CN115626837B - Heat-insulating energy-saving material for building and preparation method thereof - Google Patents

Heat-insulating energy-saving material for building and preparation method thereof Download PDF

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CN115626837B
CN115626837B CN202211530675.8A CN202211530675A CN115626837B CN 115626837 B CN115626837 B CN 115626837B CN 202211530675 A CN202211530675 A CN 202211530675A CN 115626837 B CN115626837 B CN 115626837B
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fiber
polyvinyl alcohol
parts
carrying
preparation
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CN115626837A (en
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陈磊
仲华
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Suzhou Huilin Energy Saving Material Co ltd
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Abstract

The invention discloses a heat-insulating energy-saving material for buildings and a preparation method thereof, wherein a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate are used as raw materials, fibers are obtained by spinning, and hollow micro-nanofibers are obtained by calcining; and then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, shearing the pretreated fiber at a high speed to prepare a fiber filler, and roasting, foaming and pore-forming the pretreated fiber by using sericite powder, coal gangue, magnesium carbonate, nano silicon carbide whiskers, a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, a polyvinyl alcohol aqueous solution and the like as raw materials. The material has the advantages of good heat insulation effect, excellent mechanical property and long service life.

Description

Heat-insulating energy-saving material for building and preparation method thereof
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a heat-insulating energy-saving material for buildings and a preparation method thereof.
Background
With the global problems of exhaustion of fossil energy and environmental pollution, how to improve the energy utilization efficiency and develop renewable energy has become an important issue facing human beings. Most of the buildings at present belong to non-energy-saving buildings with high energy consumption, and during the use period, a large amount of energy is consumed by air conditioners, heating, hot water supply and the like, and especially the heat energy loss caused by poor heat insulation accounts for a very large proportion. Therefore, the development of the heat-insulating and energy-saving material has very important significance for reducing energy consumption of buildings.
In order to realize heat preservation and energy conservation, the most common method at home and abroad at present is to apply a heat preservation and thermal insulation layer on an outer wall and an inner wall, so that heat radiation is prevented from being transmitted to the inside of a room in hot summer, and indoor higher temperature is prevented from being transmitted to the outside of the cold room in cold winter. Common heat-insulating layer materials in the market can be divided into two categories, namely high-molecular organic materials and inorganic materials. Expanded polystyrene foam boards, crosslinked polyethylene foam boards and foamed polyurethane boards are common high molecular organic materials, and foamed cement boards and the like belong to inorganic materials. The main advantages of the high molecular organic material are good toughness, light weight, high heat insulation efficiency, poor fire resistance, easy ignition after ignition, serious danger to life safety, poor aging resistance, short service life, complex installation procedure and high cost. The inorganic material has the main advantages of low cost, flame retardancy, good aging resistance, easy installation and obvious defects, can increase the integral weight of a building, and is lack of toughness.
Taking the most common insulation board at present as an example, the preparation method comprises the following steps: polystyrene resin as material, other supplementary material and polymer are heated, mixed, injected with catalyst and extruded to form rigid foamed plastic board. The heat-insulating board has the moisture-proof and waterproof performances, and can reduce the thickness of an outer enclosure structure of a building, thereby increasing the indoor use area. However, stress concentration is easy to occur on the plate, and the plate is easy to damage and crack; the air permeability is poor, if the temperature difference between the two sides of the plate is large, the humidity is high, the plate is easy to dew, the plate is not firmly bonded with plastering mortar, the plate is easy to fall off, and the outer tile can fall off more quickly and seriously. Further, the service life is limited, and it is difficult to apply the steel sheet to a high-rise building where high strength is required.
The patent CN215106171U discloses a building energy-saving heat-insulating material, which comprises a base layer, wherein the left side plate and the right side plate of the base layer are both bonded with sound-insulating layers, a decorative layer is bonded on the sound-insulating layer on the left side, and a heat-insulating layer, a flame-retardant layer and a decorative layer are sequentially bonded on the sound-insulating layer on the right side from left to right; the flame-retardant layer comprises a first flame-retardant layer made of PE (polyethylene) fabric and a second flame-retardant layer made of aluminum foil, the first flame-retardant layer is bonded on the heat-insulating layer, and the second flame-retardant layer is bonded on the first flame-retardant layer; evenly be provided with a plurality of archs on the curb plate about the basic unit, the puigging corresponds the position with the arch and has seted up the recess on the curb plate towards the basic unit, and the arch corresponds to peg graft in the recess. This patent technology relates to through multilayer structure and realizes corresponding function, and the risk that drops is big, and life can't guarantee at all.
Patent application CN106836531A discloses a novel heat-preservation energy-saving building material, which is formed by bonding a magnesium oxychloride internal and external wall heat-preservation heat-insulation fireproof material plate and an external decorative plate calcium magnesium silicate decorative plate (or a metal aluminum decorative plate) by using a fireproof adhesive epoxy resin through composite pressurization. The heat preservation effect of the patent technology is general.
Patent application CN103524078A discloses an energy-saving heat-insulating material for building walls, which is composed of the following components in parts by weight: 40 parts of open-cell expanded perlite, 30 parts of diatomite, 3-8 parts of open-cell expanded perlite, 3-6 parts of lubricant, 1-9 parts of crosslinking modifier, 1-3 parts of filler, 2-4 parts of flame retardant, 1-5 parts of ash, 2-9 parts of diatomite, 0.5-3.5 parts of mica powder and 4 parts of hydroxyethyl cellulose. The patent technology utilizes various inorganic fillers, and the prepared wall material has good heat insulation effect, is environment-friendly and is simple and convenient to prepare. However, the main problem of the technology of the patent is that the open-pore expanded perlite has high water absorption rate, and the shrinkage occurs due to water loss in the setting and hardening processes, so that the heat insulation performance is obviously reduced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a heat-insulating energy-saving material for buildings and a preparation method thereof, and the heat-insulating energy-saving material has the advantages of good heat-insulating effect, excellent mechanical property and long service life.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then, taking sericite powder and coal gangue as raw materials, adding magnesium carbonate and nano silicon carbide whiskers as additives, uniformly mixing, adding a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, a polyvinyl alcohol aqueous solution with the concentration of 6-10 wt% and a fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and forming pores, and naturally cooling to room temperature to obtain the composite material;
the phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2 to 3: 1-2 are evenly mixed to obtain; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
Preferably, the polymerization reaction liquid is prepared by the following method in parts by weight: firstly, adding 200-210 parts of methyl vinyl dichlorosilane, 15-20 parts of polyvinyl alcohol-400 and 5-6 parts of ammonium persulfate into 700-800 parts of deionized water, uniformly stirring, adjusting the pH =7, slowly adding 400-420 parts of methyl methacrylate, 80-100 parts of isooctyl acrylate and 40-50 parts of methacrylic acid while stirring, heating to 80-90 ℃ after the feeding is finished, and keeping the temperature and stirring for 120-140 minutes.
Preferably, in the step (1), the fiber is obtained by the following preparation method in parts by weight: firstly, adding 5-6 parts of yttrium nitrate hexahydrate and 2-3 parts of zirconium oxychloride octahydrate into 10-11 parts of polyvinyl alcohol solution, uniformly stirring to obtain spinning solution, then adopting a jet spinning method to spray the spinning solution from a spinning nozzle at a rate of 8-10 mL/h, and depositing the obtained fibers on a receiver which is 50-70 cm away from the spinning nozzle.
Preferably, in the step (1), the polyvinyl alcohol solution is prepared by dissolving polyvinyl alcohol in deionized water 9-10 times the weight of the polyvinyl alcohol.
Preferably, in the step (1), the calcination process conditions are as follows: heating to 800-900 ℃ at the speed of 5-8 ℃/min, carrying out heat preservation calcination for 5-6 hours, heating to 1050-1150 ℃ at the speed of 2-3 ℃/min, and carrying out heat preservation calcination for 1-2 hours.
Preferably, in the step (2), the mass ratio of the hollow micro-nanofiber to the phase-change material liquid to the polymerization reaction liquid is 10: 50-60: 55 to 65.
Preferably, in the step (2), the process conditions of the dipping treatment are as follows: dipping for 2-3 hours under the ultrasonic oscillation of 300-400W.
Preferably, in the step (2), the mass ratio of the pretreated fiber to the ethyl acetate is 1: 5-6, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 3000-4000 r/min, and the treatment time is 60-70 minutes.
Preferably, in the step (3), the mass ratio of the sericite powder, the coal gangue, the magnesium carbonate, the nano silicon carbide whisker, the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, the polyvinyl alcohol aqueous solution and the fiber filler is 70-80: 20 to 30:2 to 3:4 to 5:4 to 5:20 to 30:8 to 10.
Preferably, in the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle diameter is 80-100 nm.
Preferably, in the step (3), the ball milling process conditions are as follows: the ball milling speed is 200-300 ℃/min, and the ball milling time is 50-60 minutes.
Preferably, in the step (3), the process conditions for roasting, foaming and pore-forming are as follows: heating to 500-600 ℃ at the speed of 2-3 ℃/min, preserving heat for 2-3 hours, then heating to 1200-1300 ℃ at the speed of 6-8 ℃/min, and preserving heat for 2-3 hours.
The invention also claims a heat-insulating energy-saving material for buildings, which is obtained by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers; and then carrying out dipping treatment on the hollow micro-nano fibers by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fibers by using a polymerization reaction liquid after separation, separating to obtain pretreated fibers, shearing the pretreated fibers at a high speed to prepare a fiber filler, and roasting, foaming and pore-forming the raw materials by using sericite powder, coal gangue, magnesium carbonate, nano silicon carbide whiskers, a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, a polyvinyl alcohol aqueous solution and the like to obtain the heat-insulating and energy-saving material for the building. The material has the advantages of good heat insulation effect, excellent mechanical property and long service life. The specific analysis is as follows:
1. firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain the hollow micro-nanofiber. The hollow micro-nano fiber has a reinforcing effect, improves the mechanical property of a product, has a large specific surface area, has a hollow structure, has a certain heat preservation and insulation effect, and fully adsorbs phase-change material liquid and polymerization reaction liquid in the subsequent process, so that the heat preservation effect of the product is further improved.
2. And (3) carrying out impregnation treatment on the hollow micro-nano fibers by using a phase change material liquid and a polymerization reaction liquid in sequence, and preparing the fiber filler by high-speed shearing. The sequence of the dipping treatment can not be reversed, a polymer layer can be formed after the polymerization reaction liquid is dipped, and the service life of the product is prolonged due to the further improvement of the heat insulation performance and the mechanical property.
3. The invention takes sericite powder and coal gangue as raw materials, magnesium carbonate and nano silicon carbide crystal whisker are added as additives, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, polyvinyl alcohol aqueous solution and fiber filler are added after uniform mixing, the slurry is prepared by uniform ball milling, the slurry is filled into a mould, and the roasting, foaming and pore-forming are carried out. The process forms a very rich pore channel structure, and the polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer is volatilized under the calcining condition to form a microporous structure, so that the heat insulation performance of the product is greatly improved, the mechanical property is not influenced, and the service life of the product is prolonged.
4. The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2 to 3: 1-2, and the heat preservation performance of the product is obviously improved through the synergistic effect of the three components.
5. The polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid. The polymerization reaction liquid has a surface modification effect, further improves the heat insulation performance and the mechanical property of the product, and prolongs the service life of the product.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
All commodities are purchased through market channels in the invention unless specially stated.
Example 1
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then taking 70g of sericite powder and 20g of coal gangue as raw materials, adding 2g of magnesium carbonate and 4g of nano silicon carbide whisker as additives, uniformly mixing, adding 4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 20g of polyvinyl alcohol aqueous solution with the concentration of 6wt% and 8g of fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the composite material.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2:1, uniformly mixing to obtain the product; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 200g of methyl vinyl dichlorosilane, 15g of polyvinyl alcohol-400 and 5g of ammonium persulfate into 700g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 400g of methyl methacrylate, 80g of isooctyl acrylate and 40g of methacrylic acid at a constant speed while stirring, feeding for 30 minutes, heating to 80 ℃ after feeding is finished, and keeping the temperature and stirring for 120 minutes to obtain the acrylic acid modified acrylic acid.
In the step (1), the fiber is obtained by the following preparation method: firstly, 5g of yttrium nitrate hexahydrate and 2g of zirconium oxychloride octahydrate are added into 10g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at a rate of 8mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 50cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in deionized water 9 times of the weight of the polyvinyl alcohol.
The calcination process conditions are as follows: heating to 800 ℃ at the speed of 5 ℃/min, carrying out heat preservation calcination for 5 hours, then heating to 1050 ℃ at the speed of 2 ℃/min, and carrying out heat preservation calcination for 1 hour.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:50:55.
the process conditions of the dipping treatment are as follows: immersing the substrate in 300W ultrasonic wave for 2 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:5, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 3000r/min, and the treatment time is 60 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 80nm.
The process conditions of ball milling are as follows: the ball milling speed is 200 ℃/min, and the ball milling time is 50 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 500 deg.C at 2 deg.C/min, holding for 2 hr, heating to 1200 deg.C at 6 deg.C/min, and holding for 2 hr.
Example 2
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then, 80g of sericite powder and 30g of coal gangue are used as raw materials, 3g of magnesium carbonate and 5g of nano silicon carbide whiskers are added as additives, after uniform mixing, 5g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 30g of polyvinyl alcohol aqueous solution with the concentration of 10wt% and 10g of fiber filler are added, uniform ball milling is carried out to prepare slurry, the slurry is filled into a mold, the mold is roasted, foamed and pore-formed, and the mixture is naturally cooled to room temperature, so that the high-performance composite material is obtained.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:3:2, uniformly mixing to obtain the mixture; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 210g of methyl vinyl dichlorosilane, 20g of polyvinyl alcohol-400 and 6g of ammonium persulfate into 800g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 420g of methyl methacrylate, 100g of isooctyl acrylate and 50g of methacrylic acid at a constant speed while stirring, feeding for 40 minutes, heating to 90 ℃ after feeding is finished, and keeping the temperature and stirring for 140 minutes to obtain the modified polyvinyl chloride.
In the step (1), the fiber is obtained by the following preparation method: firstly, 6g of yttrium nitrate hexahydrate and 3g of zirconium oxychloride octahydrate are added into 11g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at the speed of 10mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 70cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in 10 times of deionized water.
The calcination process conditions are as follows: heating to 900 ℃ at the speed of 8 ℃/min, carrying out heat preservation calcination for 6 hours, then heating to 1150 ℃ at the speed of 3 ℃/min, and carrying out heat preservation calcination for 2 hours.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:60:65.
the process conditions of the dipping treatment are as follows: immersing the substrate in 400W ultrasonic wave for 3 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:6, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 4000r/min, and the treatment time is 70 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 100nm.
The process conditions of ball milling are as follows: the ball milling speed is 300 ℃/min, and the ball milling time is 60 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 600 deg.C at 3 deg.C/min, maintaining for 3 hr, heating to 1300 deg.C at 8 deg.C/min, and maintaining for 3 hr.
Example 3
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then taking 70g of sericite powder and 30g of coal gangue as raw materials, adding 2g of magnesium carbonate and 5g of nano silicon carbide whisker as additives, uniformly mixing, adding 4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 30g of polyvinyl alcohol aqueous solution with the concentration of 6wt% and 10g of fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the composite material.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2:2, uniformly mixing to obtain the mixture; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 210g of methyl vinyl dichlorosilane, 15g of polyvinyl alcohol-400 and 6g of ammonium persulfate into 700g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 400g of methyl methacrylate, 100g of isooctyl acrylate and 40g of methacrylic acid at a constant speed while stirring, feeding for 40 minutes, heating to 80 ℃ after feeding is finished, and keeping the temperature and stirring for 140 minutes to obtain the modified polyvinyl chloride.
In the step (1), the fiber is obtained by the following preparation method: firstly, 5g of yttrium nitrate hexahydrate and 3g of zirconium oxychloride octahydrate are added into 10g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at a rate of 10mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 50cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in 10 times of deionized water.
The calcination process conditions are as follows: heating to 900 ℃ at the speed of 5 ℃/min, keeping the temperature and calcining for 5 hours, then heating to 1050 ℃ at the speed of 3 ℃/min, keeping the temperature and calcining for 2 hours.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:50:65.
the process conditions of the dipping treatment are as follows: immersing the substrate in 300W ultrasonic wave for 3 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:5, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 4000r/min, and the treatment time is 60 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 100nm.
The process conditions of ball milling are as follows: the ball milling speed is 200 ℃/min, and the ball milling time is 60 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 600 deg.C at 2 deg.C/min, holding for 2 hr, heating to 1200 deg.C at 8 deg.C/min, and holding for 3 hr.
Example 4
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then, 80g of sericite powder and 20g of coal gangue are used as raw materials, 3g of magnesium carbonate and 4g of nano silicon carbide whisker are added as additives, after uniform mixing, 5g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 20g of polyvinyl alcohol aqueous solution with the concentration of 10wt% and 8g of fiber filler are added, slurry is prepared by uniform ball milling, the slurry is filled into a mold, the mold is roasted, foamed and pore-formed, and the mixture is naturally cooled to room temperature, so that the high-performance composite material is obtained.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:3:1, uniformly mixing to obtain the product; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 200g of methyl vinyl dichlorosilane, 20g of polyvinyl alcohol-400 and 5g of ammonium persulfate into 800g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 420g of methyl methacrylate, 80g of isooctyl acrylate and 50g of methacrylic acid at a constant speed while stirring, feeding for 30 minutes, heating to 90 ℃ after feeding is finished, and keeping the temperature and stirring for 120 minutes to obtain the modified polyvinyl chloride.
In the step (1), the fiber is obtained by the following preparation method: firstly, 6g of yttrium nitrate hexahydrate and 2g of zirconium oxychloride octahydrate are added into 11g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at a rate of 8mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 70cm away from the spinning nozzle.
The polyvinyl alcohol solution is prepared by dissolving polyvinyl alcohol in deionized water 9 times of the weight of the polyvinyl alcohol.
The calcining process conditions are as follows: heating to 800 ℃ at the speed of 8 ℃/min, carrying out heat preservation calcination for 6 hours, then heating to 1150 ℃ at the speed of 2 ℃/min, and carrying out heat preservation calcination for 1 hour.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:60: 55.
the process conditions of the dipping treatment are as follows: immersing the substrate in 400W ultrasonic wave for 2 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:6, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 3000r/min, and the treatment time is 70 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 80nm.
The process conditions of ball milling are as follows: the ball milling speed is 300 ℃/min, and the ball milling time is 50 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 500 deg.C at 3 deg.C/min, maintaining for 3 hr, heating to 1300 deg.C at 6 deg.C/min, and maintaining for 2 hr.
Example 5
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then, taking 75g of sericite powder and 25g of coal gangue as raw materials, adding 2.5g of magnesium carbonate and 4,5g of nano silicon carbide whisker as additives, uniformly mixing, adding 4.5g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 25g of polyvinyl alcohol aqueous solution with the concentration of 8wt% and 9g of fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the nano silicon carbide ceramic.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2.5:1.5, evenly mixing to obtain the product; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: firstly, adding 205g of methyl vinyl dichlorosilane, 18g of polyvinyl alcohol-400 and 5.5g of ammonium persulfate into 750g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 410g of methyl methacrylate, 90g of isooctyl acrylate and 45g of methacrylic acid at a constant speed while stirring, feeding for 35 minutes, heating to 85 ℃ after feeding is finished, and stirring for 130 minutes under heat preservation.
In the step (1), the fiber is obtained by the following preparation method: firstly, adding 5.5g of yttrium nitrate hexahydrate and 2.5g of zirconium oxychloride octahydrate into 10.5g of polyvinyl alcohol solution, uniformly stirring to obtain a spinning solution, then adopting a jet spinning method to spray the spinning solution from a spinning nozzle at a rate of 9mL/h, and depositing the obtained fibers on a receiver 60cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in 10 times of deionized water.
The calcination process conditions are as follows: heating to 850 ℃ at the speed of 7 ℃/min, carrying out heat preservation calcination for 5.5 hours, then heating to 1100 ℃ at the speed of 2.5 ℃/min, and carrying out heat preservation calcination for 1.5 hours.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:55:60.
the process conditions of the dipping treatment are as follows: the mixture was immersed in 400W ultrasonic waves for 2.5 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:5.5, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 4000r/min, and the treatment time is 65 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 90nm.
The process conditions of ball milling are as follows: the ball milling speed is 250 ℃/min, and the ball milling time is 55 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 550 deg.C at 2.5 deg.C/min, maintaining for 2.5 hr, heating to 1250 deg.C at 7 deg.C/min, and maintaining for 2.5 hr.
Comparative example 1
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps: taking 70g of sericite powder and 20g of coal gangue as raw materials, adding 2g of magnesium carbonate and 4g of nano silicon carbide whisker as additives, uniformly mixing, adding 4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer and 20g of 6wt% polyvinyl alcohol aqueous solution, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the nano silicon carbide/mica composite material.
Wherein, the length-diameter ratio of the nanometer silicon carbide crystal whisker is 15:1, the particle size is 80nm.
The process conditions of ball milling are as follows: the ball milling speed is 200 ℃/min, and the ball milling time is 50 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 500 deg.C at 2 deg.C/min, holding for 2 hr, heating to 1200 deg.C at 6 deg.C/min, and holding for 2 hr.
Comparative example 2
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then, carrying out immersion treatment on the hollow micro-nanofiber by using a phase-change material liquid, separating, then carrying out immersion treatment by using a polymerization reaction liquid, and separating to obtain a pretreated fiber;
(3) Then taking 70g of sericite powder and 20g of coal gangue as raw materials, adding 2g of magnesium carbonate and 4g of nano silicon carbide whisker as additives, uniformly mixing, adding 4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 20g of 6wt% polyvinyl alcohol aqueous solution with the concentration of 8g of pretreatment fibers, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the nano silicon carbide/titanium dioxide composite material.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2:1, uniformly mixing to obtain the product; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 200g of methyl vinyl dichlorosilane, 15g of polyvinyl alcohol-400 and 5g of ammonium persulfate into 700g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 400g of methyl methacrylate, 80g of isooctyl acrylate and 40g of methacrylic acid at a constant speed while stirring, feeding for 30 minutes, heating to 80 ℃ after feeding is finished, and stirring for 120 minutes under heat preservation.
In the step (1), the fiber is obtained by the following preparation method: firstly, 5g of yttrium nitrate hexahydrate and 2g of zirconium oxychloride octahydrate are added into 10g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at a rate of 8mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 50cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in deionized water 9 times of the weight of the polyvinyl alcohol.
The calcination process conditions are as follows: heating to 800 ℃ at the speed of 5 ℃/min, carrying out heat preservation calcination for 5 hours, then heating to 1050 ℃ at the speed of 2 ℃/min, and carrying out heat preservation calcination for 1 hour.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:50:55.
the process conditions of the dipping treatment are as follows: the substrate was immersed in 300W ultrasonic waves for 2 hours.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 80nm.
The process conditions of ball milling are as follows: the ball milling speed is 200 ℃/min, and the ball milling time is 50 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 500 deg.C at 2 deg.C/min, holding for 2 hr, heating to 1200 deg.C at 6 deg.C/min, and holding for 2 hr.
Comparative example 3
A preparation method of a heat-insulating energy-saving material for buildings comprises the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fibers by using a polymerization reaction liquid, carrying out dipping treatment on the hollow micro-nano fibers by using a phase-change material liquid after separation, separating to obtain pretreated fibers, adding the pretreated fibers into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then taking 70g of sericite powder and 20g of coal gangue as raw materials, adding 2g of magnesium carbonate and 4g of nano silicon carbide whisker as additives, uniformly mixing, adding 4g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, 20g of 6wt% polyvinyl alcohol aqueous solution with the concentration of 8g of fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and pore-forming, and naturally cooling to room temperature to obtain the nano-composite material.
The phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2:1, uniformly mixing to obtain the product; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
The preparation method of the polymerization reaction liquid comprises the following steps: adding 200g of methyl vinyl dichlorosilane, 15g of polyvinyl alcohol-400 and 5g of ammonium persulfate into 700g of deionized water, uniformly stirring, adjusting the pH to be =7, slowly adding 400g of methyl methacrylate, 80g of isooctyl acrylate and 40g of methacrylic acid at a constant speed while stirring, feeding for 30 minutes, heating to 80 ℃ after feeding is finished, and stirring for 120 minutes under heat preservation.
In the step (1), the fiber is obtained by the following preparation method: firstly, 5g of yttrium nitrate hexahydrate and 2g of zirconium oxychloride octahydrate are added into 10g of polyvinyl alcohol solution and uniformly stirred to obtain spinning solution, then the spinning solution is sprayed out from a spinning nozzle at a rate of 8mL/h by adopting a jet spinning method, and the obtained fibers are deposited on a receiver which is 50cm away from the spinning nozzle.
The polyvinyl alcohol solution is obtained by dissolving polyvinyl alcohol in deionized water 9 times of the weight of the polyvinyl alcohol.
The calcination process conditions are as follows: heating to 800 ℃ at the speed of 5 ℃/min, carrying out heat preservation calcination for 5 hours, then heating to 1050 ℃ at the speed of 2 ℃/min, and carrying out heat preservation calcination for 1 hour.
In the step (2), the mass ratio of the hollow micro-nano fibers to the phase-change material liquid to the polymerization reaction liquid is 10:50:55.
the process conditions of the dipping treatment are as follows: the substrate was immersed in 300W ultrasonic waves for 2 hours.
The mass ratio of the pretreated fiber to the ethyl acetate is 1:5, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 3000r/min, and the treatment time is 60 minutes.
In the step (3), the length-diameter ratio of the nano silicon carbide whisker is 15:1, the particle size is 80nm.
The process conditions of ball milling are as follows: the ball milling speed is 200 ℃/min, and the ball milling time is 50 minutes.
The technological conditions of roasting, foaming and pore-forming are as follows: heating to 500 deg.C at a rate of 2 deg.C/min, maintaining for 2 hr, heating to 1200 deg.C at a rate of 6 deg.C/min, and maintaining for 2 hr.
The properties of the materials obtained in examples 1 to 5 and comparative examples 1 to 3 were examined.
1. Thermal insulation performance: and (3) performing a heat conductivity coefficient test by referring to GB/T10294-2008 < thermal conductivity coefficient/thermal conductivity resistance test of heat insulation materials >.
2. Mechanical properties: the compressive strength is tested by referring to GB/T5486-2008 'test method for inorganic hard heat insulation products'.
The test results are shown in Table 1.
TABLE 1 Performance test results
Figure 239402DEST_PATH_IMAGE001
As can be seen from Table 1, the materials obtained in examples 1 to 5 have good thermal insulation properties and mechanical properties, and greatly improve the service life for building thermal insulation.
The comparative example 1 omits the hollow micro-nano fiber, the comparative example 2 omits the high-speed shearing treatment of the pretreated fiber, the order of the impregnation treatment of the phase-change material liquid and the polymerization reaction liquid in the comparative example 3 is reversed, the heat preservation performance and the mechanical property of the product are both obviously improved, and the synergistic effects of the addition and the further treatment of the hollow micro-nano fiber, the control of the impregnation process and the like are demonstrated, so that the product effect is improved.
The technical idea of the present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must depend on the above embodiments to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitution of individual materials for the product of the present invention and addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. A preparation method of a heat-insulating energy-saving material for buildings is characterized by comprising the following specific steps:
(1) Firstly, taking a polyvinyl alcohol solution, yttrium nitrate hexahydrate and zirconium oxychloride octahydrate as raw materials, spinning to obtain fibers, and calcining to obtain hollow micro-nanofibers;
(2) Then carrying out dipping treatment on the hollow micro-nano fiber by using a phase-change material liquid, carrying out dipping treatment on the hollow micro-nano fiber by using a polymerization reaction liquid after separation, separating to obtain a pretreated fiber, adding the pretreated fiber into ethyl acetate, stirring and uniformly mixing, carrying out high-speed shearing treatment, carrying out spray drying, washing with water, and drying to obtain a fiber filler;
(3) Then, taking sericite powder and coal gangue as raw materials, adding magnesium carbonate and nano silicon carbide whiskers as additives, uniformly mixing, adding a polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, a polyvinyl alcohol aqueous solution with the concentration of 6-10 wt% and a fiber filler, uniformly ball-milling to prepare slurry, filling the slurry into a mold, roasting, foaming and forming pores, and naturally cooling to room temperature to obtain the composite material;
the phase-change material liquid is prepared from methyl stearate, dodecanol and liquid paraffin according to a mass ratio of 1:2 to 3: 1-2 are evenly mixed to obtain; the polymerization reaction liquid is obtained by polymerization reaction of raw materials of methyl vinyl dichlorosilane, methyl methacrylate, isooctyl acrylate and methacrylic acid.
2. The method according to claim 1, wherein the polymerization reaction solution is prepared by the following method in parts by weight: adding 200-210 parts of methyl vinyl dichlorosilane, 15-20 parts of polyvinyl alcohol-400 and 5-6 parts of ammonium persulfate into 700-800 parts of deionized water, stirring and uniformly mixing, adjusting the pH to be =7, slowly adding 400-420 parts of methyl methacrylate, 80-100 parts of isooctyl acrylate and 40-50 parts of methacrylic acid while stirring, heating to 80-90 ℃ after feeding is finished, and keeping the temperature and stirring for 120-140 minutes.
3. The production method according to claim 1, wherein in the step (1), the fiber is obtained by the following production method in parts by weight: firstly, adding 5-6 parts of yttrium nitrate hexahydrate and 2-3 parts of zirconium oxychloride octahydrate into 10-11 parts of polyvinyl alcohol solution, uniformly stirring to obtain spinning solution, then adopting a jet spinning method to spray the spinning solution from a spinning nozzle at a rate of 8-10 mL/h, and depositing the obtained fibers on a receiver which is 50-70 cm away from the spinning nozzle.
4. The preparation method according to claim 1, wherein in the step (1), the calcination process conditions are as follows: heating to 800-900 ℃ at the speed of 5-8 ℃/min, carrying out heat preservation calcination for 5-6 hours, heating to 1050-1150 ℃ at the speed of 2-3 ℃/min, and carrying out heat preservation calcination for 1-2 hours.
5. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the hollow micro-nanofiber, the phase-change material liquid and the polymerization reaction liquid is 10: 50-60: 55 to 65.
6. The method according to claim 1, wherein in the step (2), the process conditions of the dipping treatment are as follows: dipping for 2-3 hours under the ultrasonic oscillation of 300-400W.
7. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the pretreated fiber to the ethyl acetate is 1: 5-6, the process conditions of the high-speed shearing treatment are as follows: the rotating speed is 3000-4000 r/min, and the treatment time is 60-70 minutes.
8. The preparation method according to claim 1, wherein in the step (3), the mass ratio of sericite powder, coal gangue, magnesium carbonate, nano silicon carbide whisker, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, polyvinyl alcohol aqueous solution and fibrous filler is 70-80: 20 to 30:2 to 3:4 to 5:4 to 5:20 to 30:8 to 10.
9. The preparation method according to claim 1, wherein in the step (3), the process conditions for roasting, foaming and pore-forming are as follows: heating to 500-600 ℃ at the speed of 2-3 ℃/min, preserving heat for 2-3 hours, then heating to 1200-1300 ℃ at the speed of 6-8 ℃/min, and preserving heat for 2-3 hours.
10. A heat-insulating energy-saving material for buildings, which is obtained by the preparation method of any one of claims 1 to 9.
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CN109097860A (en) * 2018-07-31 2018-12-28 佛山市南海区佳妍内衣有限公司 A kind of heat storing and heat preserving functional polyurethane fiber and its manufacturing method
CN109295548A (en) * 2018-09-13 2019-02-01 南京理工宇龙新材料科技股份有限公司 A kind of zirconium oxide hollow fibre and preparation method thereof
CN111675907A (en) * 2020-05-06 2020-09-18 云南电网有限责任公司 Method for preparing high-temperature-resistant heat-insulating silicone rubber by using waste hollow fiber membranes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108585937A (en) * 2018-07-11 2018-09-28 合肥尚涵装饰工程有限公司 A kind of light-weight insulating brick of pressure resistance anticracking
CN109097860A (en) * 2018-07-31 2018-12-28 佛山市南海区佳妍内衣有限公司 A kind of heat storing and heat preserving functional polyurethane fiber and its manufacturing method
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