CN115991044B - Composite heat-insulating waterproof coiled material and production method thereof - Google Patents
Composite heat-insulating waterproof coiled material and production method thereof Download PDFInfo
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Abstract
The invention discloses a composite heat-insulating waterproof coiled material and a production method thereof, and relates to the technical field of building materials. The waterproof layer is arranged on the upper layer. In the composite heat-insulating waterproof coiled material, the heat-insulating layer comprises the following raw materials: silica aerogel, polyurethane, first polyethylene, silica-alumina molecular sieve; the waterproof layer comprises the following raw materials: asphalt, fluorosilicone oil, silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and antioxidant. The composite heat-insulating waterproof coiled material prepared by the invention integrates heat insulation, water resistance and low carbon environmental protection, and breaks through the technical bottleneck in the current market.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a composite heat-preservation waterproof coiled material and a production method thereof.
Background
The waterproof coiled material is mainly used for building walls, roofs, tunnels, highways, refuse landfills and the like, plays a role in resisting external rainwater and underground water seepage, is a flexible coiled building material product, is used as a non-leakage connection between an engineering foundation and a building, is a waterproof first barrier of the whole engineering, and plays a vital role in the whole engineering. The original waterproof coiled material is tar asphalt and petroleum asphalt paper felt, and originates from Europe and is transferred into China in the 20 th century. Along with the progress of science and technology, modern waterproof materials are rapidly developed, and the waterproof materials in China gradually trend to the 70 th century, and novel products are formulated for adapting to market demands, and coiled material products mainly comprise asphalt waterproof coiled materials and high polymer waterproof materials.
Energy conservation is the main content of the national environmental protection and energy conservation policy, and is an important component for implementing national economy sustainable development strategy. With the annual improvement of the energy-saving standard, the performance of the heat-insulating waterproof coiled material is gradually improved.
Along with the increasing standard of living, the requirements of people on air quality are also higher and higher, and green life has become a subject of attention to environment and human health. Most of the coils on the market are not focused on the development, so that the coils volatilize toxic and harmful substances during the use process to become invisible killers for human beings, the volatile organic compounds easily enter the brain through blood, the central nervous system is inhibited, headache, debilitation, drowsiness and uncomfortable feeling are caused, and many volatile organic compounds prove to be cancerogenic or suspicious cancerogenic.
In the prior art, the single performance of the coiled material is improved, and no product integrates the heat preservation, water resistance and smell of the coiled material. In view of this problem, it is necessary to develop a coil material excellent in combination properties.
Disclosure of Invention
The invention aims to provide a composite heat-insulating waterproof coiled material and a production method thereof, which are used for composite heat insulation so as to solve the problem that the heat-insulating performance and the water resistance of the existing coiled material cannot be further improved.
In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides a compound heat preservation waterproofing membrane, includes heat preservation and waterproof layer, wherein the heat preservation is in the lower floor, and the waterproof layer is on the upper strata, and the heat preservation includes following raw and other materials: silica aerogel, polyurethane, first polyethylene, silica-alumina molecular sieve; the waterproof layer comprises the following raw materials: asphalt, fluorosilicone oil, silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and antioxidant; the heat preservation layer comprises, by weight, 10-25 parts of silica aerogel, 20-40 parts of polyurethane, 50-80 parts of first polyethylene and 5-10 parts of silicon-aluminum molecular sieve; the waterproof layer comprises, by weight, 10-25 parts of asphalt, 5-15 parts of fluorosilicone oil, 5-10 parts of a silicon-aluminum molecular sieve, 60-90 parts of second polyethylene, 10-20 parts of maleic anhydride grafted polypropylene and 0.5-2 parts of an antioxidant.
Preferably, the specific surface area of the silica aerogel is 400-1000 m 2 /g。
Further preferably, the specific surface area of the silica aerogel is 600-800 m 2 /g。
The polyethylene, the silica aerogel and the polyurethane foam to form a three-dimensional network structure, so that the heat insulation material with a multi-stage honeycomb air cavity hole structure is formed, the heat insulation performance of the material can be effectively improved, and the heat insulation material has a lower heat conductivity coefficient.
Preferably, the melt mass flow rate of the polyurethane is 10-20 g/10min, the melt mass flow rate of the polyurethane being measured according to ISO 1133 using a weight of 2.16kg and at a temperature of 230 ℃.
Preferably, the melt mass flow rate of the first polyethylene is 20-40 g/10min.
Preferably, the melt mass flow rate of the second polyethylene is 0.1-15 g/10min.
The melt mass flow rates of the first and second polyethylenes are measured according to ISO 1133 using a weight of 2.16kg and at a temperature of 190 ℃.
Preferably, the fluorosilicone oil is a methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 300 to 1000 mpa.s.
Further preferably, the fluorosilicone oil is a methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 500 to 800 mpa.s.
The viscosity test of fluorosilicone oil is a measurement at 25℃using a silicone oil viscometer.
In the continuous expansion with heat and contraction with cold caused by the actual environment, the surface of the polyethylene material is quite porous, so that water molecules can permeate, and meanwhile, some impurities can be brought in, so that the polyethylene is aged in advance, and is changed from hydrophobic to hydrophilic, so that the service life of the polyethylene material is greatly shortened.
According to the invention, by adding the fluorosilicone oil, the low surface energy and super-hydrophobic characteristics of the fluorosilicone oil are utilized, so that the influence on the performance of the material is small. Mainly characterized in that the low surface energy of the fluorosilicone oil can be gathered on the surface of the material, and the super-hydrophobic characteristic can greatly reduce the wetting of the material, so that the waterproof effect of the material can be obviously improved.
The fluorosilicone oil is introduced into the polyethylene, the hydrophobic property of the material is improved through a special system, and other properties of the material are not affected, so that the obtained composition material has excellent hydrophobic property and excellent ageing resistance.
Preferably, the silicon-aluminum molecular sieve has a silicon-aluminum ratio of 20-40 in terms of the molar ratio of silicon dioxide to aluminum oxide.
The silicon-aluminum ratio can indicate the polarity degree of the molecular sieve, and the molecular sieve with high silicon-aluminum ratio presents non-polarity and has better compatibility with polyethylene. On the contrary, molecular sieves with low silica to alumina ratios exhibit polarity and poor compatibility with polyethylene.
The silicon-aluminum molecular sieve can effectively adsorb volatile organic compounds in the material, and the prepared coiled material has the characteristic of low TVOC.
Preferably, the grafting rate of maleic anhydride in the maleic anhydride grafted polypropylene is 10-20 wt.%.
Preferably, the antioxidant is a phenolic antioxidant that stops or inhibits chain initiation and chain growth reactions by capturing peroxy radicals, thereby terminating free radical chain reactions, such as: 2, 6-di-t-butyl-4-cresol, 2' -methylenebis (4-methyl-6-t-butylphenol), antioxidant 1010 and the like, and phosphite antioxidants decomposing hydroperoxides, for example: at least one of triphenyl phosphite, diphenyl-isooctyl phosphite, trilauryl phosphite, and 4,4' -p-isopropyldiphenyl C12-15-ol phosphite.
The asphalt provided by the invention can be commercially available asphalt of various types.
A production method of a composite heat-insulating waterproof coiled material comprises the following steps: preparing materials of the heat-insulating layer formula into granules by a double-screw extruder, preparing the granules into coiled materials by an extrusion and drawing process, stirring, reacting and grinding the materials of the waterproof layer formula, and preparing the coiled materials by the drawing process, wherein the heat-insulating layer is arranged on the lower layer, and the waterproof layer is arranged on the upper layer. The materials of the formula of the heat preservation layer are uniformly mixed in a high-speed mixer by adopting a one-pot mixing method, the rotating speed of the high-speed mixer is 400-600 r/min during mixing, and then the materials are prepared by a double-screw extruder, and the specific technological parameters of extrusion are as follows: the temperature of the feeding area is 170-190 ℃, the temperature of the melting area is 190-210 ℃, the temperature of the homogenizing area is 210-220 ℃, and the temperature of the die head is 200-205 ℃. The preparation process of the waterproof layer formula material comprises the following steps: adding asphalt into a stirring tank, heating to 130-140 ℃, then adding fluorosilicone oil, a silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and an antioxidant according to the weight parts of the formula, heating to 155-165 ℃ while stirring, and stirring for reacting for 0.5-1 h; and then grinding by a colloid mill or an emulsifying pump until the materials are fully and uniformly mixed.
The thickness of the prepared heat preservation layer is 5-6 mm, and the thickness of the waterproof layer is 2-3 mm.
An application of a composite heat-insulating waterproof coiled material in the field of construction.
Compared with the prior art, the invention has the beneficial effects that:
a composite heat-insulating waterproof coiled material is formed by the cooperation of polyethylene, silica aerogel and polyurethane, so that a heat-insulating material with a multi-stage honeycomb air cavity hole structure can be effectively improved in heat-insulating performance, and the heat-insulating material has a low heat conductivity coefficient. Meanwhile, the silicon-aluminum molecular sieve with the specific mole ratio of silicon dioxide to aluminum oxide is adopted, so that the characteristic of low TVOC of the coiled material is realized.
Detailed Description
The invention is further illustrated below in connection with examples which are provided solely for the purpose of illustration and are not intended to limit the scope of the invention. The experimental procedures in the examples below, without specific details, are generally performed under conditions conventional in the art or recommended by the manufacturer; the raw materials, reagents and the like used, unless otherwise specified, are those commercially available from conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art in light of the above teachings are intended to be within the scope of the invention as claimed.
Silica aerogel 1: specific surface area of 400m 2 /g, commercially available;
silica aerogel 2: specific surface area of 1000m 2 /g, commercially available;
silica aerogel 3: specific surface area of 600m 2 /g, commercially available;
silica aerogel 4: specific surface area of 800m 2 /g, commercially available;
silica aerogel 5: specific surface area of 200m 2 /g, commercially available;
fluorosilicone oil 1: methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 300 mpa.s, as measured with a silicone oil viscometer, at 25 ℃, commercially available;
fluorosilicone oil 2: methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 1000 mpa.s, measured at 25 ℃, commercially available using a silicone oil viscometer;
fluorosilicone oil 3: methyl-terminated polytrifluoropropyl silicone oils having a viscosity of 500 mpa.s, measured at 25 ℃, commercially available using a silicone oil viscometer;
fluorosilicone oil 4: methyl-terminated polytrifluoropropyl silicone oils having a viscosity of 800mpa.s, as measured with a silicone oil viscometer, at 25 ℃, commercially available;
fluorosilicone oil 5: methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 1500 mpa.s, as measured with a silicone oil viscometer, commercially available at 25 ℃;
fluorosilicone oil 6: methyl-terminated polytrifluoropropyl silicone oil having a viscosity of 200 mpa.s, as measured with a silicone oil viscometer, at 25 ℃, commercially available;
silicon-aluminum molecular sieve 1: the silicon-aluminum ratio is that the mole ratio of silicon dioxide to aluminum oxide is 20, and the silicon-aluminum ratio is commercially available;
and (2) a silicon-aluminum molecular sieve: the silicon-aluminum ratio is that the mole ratio of silicon dioxide to aluminum oxide is 40, and the silicon-aluminum ratio is commercially available;
and 3. A silicon-aluminum molecular sieve: the silicon-aluminum ratio is that the mole ratio of silicon dioxide to aluminum oxide is 10, and the silicon-aluminum ratio is commercially available; polyurethane: melt mass flow rate 15g/10min, commercially available;
first polyethylene 1: melt mass flow rate 20g/10min, commercially available;
first polyethylene 2: melt mass flow rate 40g/10min, commercially available;
second polyethylene 1: melt mass flow rate 5g/10min, commercially available;
second polyethylene 2: melt mass flow rate 15g/10min, commercially available;
maleic anhydride grafted polypropylene: the grafting ratio of maleic anhydride was 15wt.%, commercially available;
2,2' -methylenebis (4-methyl-6-tert-butylphenol), commercially available;
asphalt, 90# commercially available.
The invention relates to a production method of a composite heat-insulating waterproof coiled material heat-insulating layer material and a waterproof layer material, which are produced in an embodiment and a comparative example, and specifically comprises the following steps of preparing the heat-insulating layer material (silica aerogel, polyurethane, first polyethylene and silicon-aluminum molecular sieve) and the waterproof layer material (asphalt, fluorosilicone oil, silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and antioxidant) according to the parts by weight of each embodiment and comparative example, wherein the heat-insulating layer material comprises the following steps:
uniformly mixing materials of the formula of the heat preservation layer in a high-speed mixer by adopting a one-pot mixing method, wherein the rotating speed of the high-speed mixer is 500r/min during mixing, and then the materials are prepared by a double-screw extruder, and the specific technological parameters of extrusion are as follows: the feed zone temperature was 180 ℃, the melt zone temperature was 200 ℃, the homogenization zone temperature was 220 ℃, and the die temperature was 205 ℃.
The preparation process of the waterproof layer formula material comprises the following steps: adding asphalt into a stirring tank, heating to 140 ℃, then adding fluorosilicone oil, a silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and an antioxidant according to the weight parts of the formula, heating to 165 ℃ while stirring, and stirring for reacting for 0.5h; and then grinding by a colloid mill or an emulsifying pump until the materials are fully and uniformly mixed.
Examples 1-6 and comparative examples 1-2 heat insulation layers were prepared by mixing the materials of the heat insulation layers in a high speed mixer and then preparing the heat insulation layers by a twin screw extruder. The thermal conductivity and total organic compound emission (TVOC) carbon were measured for the heat insulation layers prepared in examples 1 to 6 and comparative examples 1 to 2, and the performance index is shown in table 1.
Examples 7-13 and comparative examples 3-4 were prepared with the raw material formulations shown in Table 2 by mixing the raw materials of the waterproof layer in a high-speed mixer and then preparing the waterproof layer by a twin-screw extruder. The compositions prepared in examples 7 to 13 and comparative examples 3 to 4 were subjected to measurement of water contact angle and total carbon of organic compound emission (TVOC), and the performance index is shown in table 2.
Aqueous contact angle: and adopting an appearance image analysis method and adopting an angle measurement method for testing.
Thermal conductivity coefficient: the measurement was carried out according to the single plate method in GB/T3399-1982 (thermal plate method for test method for thermal conductivity of plastics).
Organic compound emission (TVOC):
the granules of the heat preservation layer and the waterproof layer prepared by the method are firstly dried in a blast drying oven at 80+/-5 ℃ for 2 hours, and then are prepared on an injection molding machine according to the test standard. The test bars were adjusted at 23℃for 24 hours before testing.
Organic compound emission measurement (TVOC) was measured according to TS-INT-002.
The samples were broken into small pieces of 20mg, then 1.200.+ -. 0.0001g of the samples were weighed into headspace vials, the vials were sealed and heated at 120 ℃ for 5h, three headspace vials were made per sample in parallel. The syringe was inserted into a bottle and the volatile organics were transferred to a Gas Chromatograph (GC) under the following test conditions:
headspace conditions:
temperature: oven 120 ℃, needle tube 150 ℃ and transmission tube 180 DEG C
Time: the retention time of the needle tube is 0.35min, and the sampling is 0.5min
GC conditions:
gas chromatography oven temperature: heating at 50deg.C for 3min, heating to 200deg.C at a rate of 12deg.C/min, and maintaining the temperature at 200deg.C for 4 min;
sample inlet temperature: 200 ℃;
split ratio: 20:1
Pressure before entering the column: 10psi.
The data recorded by gas chromatography included the total peak area and the peak area of the individual species. The peak height should be more than three times of the baseline noise value, and the peak area should be more than 10% of the peak area of 0.5g acetone in 1L n-butanol solution.
The total carbon volatiles were calculated from the following formula:
E G ＝[(A a -A o )/K(G)]×2×0.6204
in the formula:
E G total carbon release in sample =
A a Total peak area of sample
A o Area of blank peak
Calibration coefficient of K (G) =acetone calibration sample
2 = coefficient related to sample mass
0.6204 Carbon content in acetone
Acetone was used as a reference substance for measuring total carbon volatilization. An amount of acetone was dissolved in 1L of n-butanol, respectively, as a calibration solution. Then 2.4. Mu.L was withdrawn from these solutions and placed in a 12mL headspace bottle. The peak area of the acetone was plotted against the concentration of the calibration solution to give a curve with a linear relationship. The slope is the calibration factor K [ K (G) is the total carbon volatilization, and K (i) is the single species volatilization ]. The equation for the calibration curve is as follows:
Y＝37.03898X+1.18222
in the formula:
y = peak area;
concentration of X=calibration sample (μg/g)
Table 1 performance test values for examples 1 to 6 and comparative examples 1 to 2
Table 2 Performance test values of examples 7 to 13 and comparative examples 3 to 4
As is clear from Table 1, examples 1 to 4 show that the heat insulating layer material obtained is excellent in heat insulating effect when the specific surface area of the silica aerogel is within the preferable range, and even more preferably when the specific surface area of the silica aerogel is 600 to 800m 2 And/g, the obtained heat preservation layer material has optimal heat preservation effect. As can be seen from example 5, when silicaAerogel having a specific surface area of 200m 2 At/g, the thermal insulation effect of the resulting thermal insulation layer material is reduced. As is clear from example 6, when the non-preferable silica-alumina molecular sieve was used, the total carbon of the obtained insulating layer material was increased. As can be seen from comparative examples 1 and 2, when a single silica aerogel was used, the thermal conductivity of the insulation material increased, indicating that the insulation was poor; when a single silicon-aluminum molecular sieve is adopted, the total carbon content of the heat-insulating layer material is increased, which indicates that the odor of the material is poor.
From examples 7 to 10, it is understood that when the viscosity of the fluorosilicone oil is within the preferable range of 300 to 800mpa.s, the waterproof property of the waterproof layer material is excellent (represented by the smaller contact angle, specifically, the smaller the contact angle is, the stronger the hydrophilicity is, the first to be wettable by water, that is, the hydrophilicity is, the larger the contact angle is, the smaller the hydrophilicity is (when other conditions are unchanged), the better the compatibility between the surface and water is indicated, and when the viscosity is further preferable of 300 to 800mpa.s, the performance of the waterproof layer is optimal. As is clear from examples 11 to 12, the properties of the waterproof layer were degraded when the viscosity of the fluorosilicone oil was not in the preferred range. As is clear from example 13, when the non-preferable silica-alumina molecular sieve is used, the total carbon content of the waterproof layer is increased. As can be seen from comparative example 3, the waterproof performance of the waterproof layer is remarkably reduced when the single fluorosilicone oil is adopted, and as can be seen from comparative example 4, the total carbon content of the waterproof layer is remarkably increased when the single silicon-aluminum molecular sieve is adopted.
The foregoing description of the embodiments of the present invention clearly and fully describes the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Although embodiments of the present invention have been described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations may be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The composite heat-insulating waterproof coiled material comprises a heat-insulating layer and a waterproof layer, wherein the heat-insulating layer is arranged on the lower layer, and the waterproof layer is arranged on the upper layer, and the composite heat-insulating waterproof coiled material is characterized in that the formula of the heat-insulating layer comprises the following raw materials: silica aerogel, polyurethane, first polyethylene, silica-alumina molecular sieve; the waterproof layer formula comprises the following raw materials: asphalt, fluorosilicone oil, silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and antioxidant; the formula of the heat preservation layer comprises, by weight, 10-25 parts of silica aerogel, 20-40 parts of polyurethane, 50-80 parts of first polyethylene and 5-10 parts of silicon-aluminum molecular sieve; the waterproof layer formula comprises, by weight, 10-25 parts of asphalt, 5-15 parts of fluorosilicone oil, 5-10 parts of a silicon-aluminum molecular sieve, 60-90 parts of second polyethylene, 10-20 parts of maleic anhydride grafted polypropylene and 0.5-2 parts of an antioxidant; the silicon-aluminum molecular sieve has a silicon-aluminum ratio of 20-40 of the mole ratio of silicon dioxide to aluminum oxide; the specific surface area of the silica aerogel is 400-1000 m 2 /g; the fluorosilicone oil is methyl-terminated polytrifluoropropyl silicone oil with the viscosity of 300-1000 mPa.s.
2. The composite heat-insulating waterproof coiled material according to claim 1, wherein the melt mass flow rate of polyurethane is 10-20 g/10min, and the melt mass flow rate of polyurethane is measured according to ISO 1133 by using a weight of 2.16kg at a temperature of 230 ℃.
3. The composite heat-insulating waterproof coiled material according to claim 1, wherein the melt mass flow rate of the first polyethylene is 20-40 g/10min, the melt mass flow rate of the second polyethylene is 0.1-15 g/10min, and the melt mass flow rates of the first polyethylene and the second polyethylene are measured according to ISO 1133 by using a weight of 2.16kg at a temperature of 190 ℃.
4. The composite heat-insulating waterproof coiled material according to claim 1, wherein the grafting rate of maleic anhydride in the maleic anhydride grafted polypropylene is 10-20wt%.
5. The composite heat-insulating waterproof coiled material according to claim 1, wherein the thickness of the heat-insulating layer is 5-6 mm, and the thickness of the waterproof layer is 2-3 mm.
6. The production method of the composite heat-insulating waterproof coiled material according to any one of claims 1 to 5, which is characterized by comprising the following steps: preparing materials of the heat-insulating layer formula into granules by a double-screw extruder, preparing the granules into coiled materials by an extrusion and drawing process, stirring, reacting and grinding the materials of the waterproof layer formula, and preparing the coiled materials by the drawing process; wherein the heat preservation layer is arranged on the lower layer, and the waterproof layer is arranged on the upper layer.
7. The production method of the composite heat-insulating waterproof coiled material according to claim 6, wherein the materials of the heat-insulating layer formula are uniformly mixed in a high-speed mixer by adopting a one-pot mixing method, the rotating speed of the high-speed mixer is 400-600 r/min during mixing, and then the composite heat-insulating waterproof coiled material is prepared by a double-screw extruder, and the specific technological parameters of extrusion are as follows: the temperature of the feeding area is 170-190 ℃, the temperature of the melting area is 190-210 ℃, the temperature of the homogenizing area is 210-220 ℃, and the temperature of the die head is 200-205 ℃; the preparation process of the waterproof layer formula material comprises the following steps: adding asphalt into a stirring tank, heating to 130-140 ℃, then adding fluorosilicone oil, a silicon-aluminum molecular sieve, second polyethylene, maleic anhydride grafted polypropylene and an antioxidant according to the weight parts of the formula, heating to 155-165 ℃ while stirring, and stirring for reacting for 0.5-1 h; and then grinding by a colloid mill or an emulsifying pump until the materials are fully and uniformly mixed.
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| CN113668258A (en) * | 2021-08-29 | 2021-11-19 | 钟小琼 | Environment-friendly flame-retardant modified asphalt waterproof coiled material and preparation method thereof |
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