CN111875870A - Aging-resistant TPO building waterproof coiled material and preparation method thereof - Google Patents
Aging-resistant TPO building waterproof coiled material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides an anti-aging TPO building waterproof coiled material and a preparation method thereof, wherein the preparation process comprises the following steps: wetting an aging resistant agent with acetone, uniformly dispersing the aging resistant agent, an emulsifier, a surfactant and water to obtain emulsion, slowly adding a calcium chloride solution to obtain a precursor emulsion, spraying a sodium carbonate solution into the precursor emulsion, stirring, standing, centrifugally separating, drying to obtain a microcapsule aging resistant agent, uniformly mixing the microcapsule aging resistant agent with a copolymer TPO resin, a flame retardant, a dispersing agent and a filler to obtain a TPO waterproof coiled material raw material, and then performing melt plasticizing extrusion, calendaring, cooling, deviation correction, edge cutting, cutting and rolling to obtain the TPO waterproof coiled material. The microcapsule aging resistant agent with the aging resistant agent as the core and the calcium carbonate as the shell structure improves the strength and the heat resistance of the aging resistant agent, meanwhile, the microcapsule aging resistant agent can be uniformly dispersed into the TPO waterproof coiled material, the calcium carbonate shell structure does not influence other properties of the coiled material, and the obtained waterproof coiled material has good mechanical property and stability and excellent aging resistance.
Description
Technical Field
The invention relates to the technical field of building waterproof materials, in particular to an anti-aging TPO building waterproof coiled material and a preparation method thereof.
Background
TPO waterproofing membrane is thermoplastic polyolefin waterproofing membrane, is with adopting advanced polymerization technique to combine together ethylene propylene rubber and polypropylene Thermoplastic Polyolefin (TPO) synthetic resin as the base stock, adds the novel waterproofing membrane that antioxidant, antiager, softener were made, can make enhancement mode waterproofing membrane with polyester fiber net check cloth as inside reinforcing material, belongs to synthetic polymer waterproofing membrane class waterproof product.
The TPO waterproof coiled material integrates the performance advantages of EPDM and PVC, and has the weather resistance, low-temperature flexibility and weldability of the latter. The material is different from the traditional plastic, shows high elasticity of rubber at normal temperature, and can be molded like plastic at high temperature. Therefore, the material has good processing performance and mechanical property, and has high-strength welding performance. And after a layer of polyester fiber fabric is additionally arranged between two layers of TPO materials, the physical properties of the TPO materials can be enhanced, and the breaking strength, fatigue resistance and puncture resistance of the TPO materials can be improved. In practical application, the product has the comprehensive characteristics of ageing resistance, high tensile strength, large elongation, construction of wet roofs, no need of a protective layer for exposure, convenience in construction, no pollution and the like, and is very suitable for being used as a waterproof layer of light energy-saving roofs, large-scale plants and environment-friendly buildings.
TPO waterproofing roll products are often used in construction or plumbing waterproofing, for waterproofing, insulating, or sound absorbing, noise reducing, etc. of buildings, which are also ubiquitous in our lives, in addition to construction applications. However, the TPO waterproofing membrane is easily aged due to environmental influences or excessively high construction temperature. At present, an anti-aging agent is added into a coil, but due to the harsh environment and the improper welding technology in the using process, an antioxidant, an ultraviolet absorbent, a photo-thermal stabilizer and the like in a TPO coil formula system are exhausted prematurely, so that the phenomena of fading, discoloration, surface gloss loss, even microcracks, hairline cracks and the like occur to a product, and the expected service life of the product is greatly shortened. The anti-aging agent is granulated to slow down consumption, but the dispersibility is poor, and the high-temperature melting process can also influence the granulation form, so that the effect of durable anti-aging can not be achieved.
The Chinese invention patent application No. 201510093221.2 discloses a waterproof coiled material and a preparation method thereof, which can solve the problems of fading, discoloration, surface gloss loss, micro-cracks, hairline cracks and the like in the use process of the existing TPO coiled material product; the waterproof coiled material comprises a thermoplastic polyolefin coiled material layer, wherein the raw materials of the thermoplastic polyolefin coiled material layer comprise a polymerization type thermoplastic polyolefin resin and a granulation auxiliary agent; the granulation auxiliary agent comprises an antioxidant, a light stabilizer and an ultraviolet absorbent, and the particle size of the granulation auxiliary agent is 0.5-1.5 mm. Chinese patent application No. 201310457103.6 discloses a TPO waterproof roll, which comprises the following components by weight: POE40-60 parts, LDPE15-35 parts, light calcium carbonate 25-27 parts, ultraviolet absorbent 0.1-1.5 parts, main antioxidant 0.1-0.5 part, auxiliary antioxidant 0.2-0.8 part, stearic acid 0.2-0.5 part and titanium dioxide 2.0-5.0 parts.
In order to avoid TPO waterproofing membrane to lead to ageing because of environmental impact or construction temperature, guarantee to maintain lasting ageing-resistant effect simultaneously, it is necessary to provide a novel ageing-resistant TPO building waterproofing membrane, and then improves TPO waterproofing membrane's ageing resistance, promotes TPO waterproofing membrane's development and application.
Disclosure of Invention
Aiming at the problem that the conventional TPO waterproof coiled material is easy to age, and the problems that the powdery or granulated anti-aging agent is easy to consume and the granular state is easy to damage when the TPO is prepared into the waterproof coiled material through melt plasticizing extrusion in the prior art, the invention provides the anti-aging TPO building waterproof coiled material and the preparation method thereof, so that the effect of lasting aging resistance of the TPO waterproof coiled material is achieved.
In order to solve the problems, the invention adopts the following technical scheme:
an aging-resistant TPO building waterproof coiled material is prepared by wetting an aging resistant agent with acetone, uniformly dispersing the wetting agent with an emulsifier, a surfactant and water to obtain an emulsion, slowly adding a calcium chloride solution to obtain a precursor emulsion, spraying a sodium carbonate solution into the precursor emulsion, stirring, standing, centrifugally separating and drying to obtain a microcapsule aging resistant agent, uniformly mixing the microcapsule aging resistant agent with a copolymer TPO resin, a flame retardant, a dispersing agent and a filler to obtain a TPO waterproof coiled material raw material, and then performing melt plasticizing extrusion, calendaring, cooling, deviation correction, edge cutting, cutting and rolling.
Preferably, the aging resistant agent is an antioxidant and a light stabilizer in a mass ratio of 1: 1-2.
More preferably, the antioxidant is one or a combination of two of basf 1010 and basf 168, and the light stabilizer is one or a combination of two of basf 2020 and 622 SF.
Preferably, the emulsifier is one of tween 80 and tween 20.
Preferably, the surfactant is an anionic surfactant.
Further preferably, the anionic surfactant is one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium oleoyloxy ethyl sulfonate.
Preferably, the copolymeric TPO resin is a polymer of ethylene and an alpha-olefin.
Further preferably, the polymer of ethylene and α -olefin is Engage8150 manufactured by Dow corporation.
Preferably, the flame retardant is stearic acid surface-modified magnesium hydroxide.
Preferably, the dispersant is polyethylene wax.
Preferably, the filler is one of light calcium carbonate and magnesium aluminum hydrotalcite.
Further preferably, the fineness of the filler is 200-300 mesh sieve.
Preferably, the mass fraction of the calcium chloride solution is 10-20%.
Preferably, the mass fraction of the sodium carbonate solution is 10-20%.
The invention also provides a preparation method of the aging-resistant TPO building waterproof coiled material, which comprises the following steps:
(1) adding an emulsifier and a surfactant into water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing the aging-resistant agent uniformly, dripping a small amount of acetone for wetting, then adding the acetone into the mixed solution, and dispersing uniformly at a stirring speed of 300-500r/min to obtain an emulsion;
(2) slowly dripping the calcium chloride solution into the emulsion, and continuously stirring for 1-3h to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution into a precursor emulsion containing a calcium chloride solution through an atomizing spray gun, so that the sodium carbonate enters the precursor emulsion in uniform small droplets, forming a uniform calcium carbonate coating layer on the surface of the anti-aging agent, continuously stirring for 0.5-2h, standing for 5-7h, performing centrifugal separation, and drying in an oven at the temperature of 40-50 ℃ to obtain the microcapsule anti-aging agent;
(4) adding the copolymerized TPO resin, the microcapsule aging resistant agent, the flame retardant, the dispersing agent and the filler into a high-speed stirrer, and uniformly mixing to obtain a TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material to a screw extruder for melt plasticizing extrusion, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then cooling, correcting, trimming, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Preferably, in the preparation of the emulsion in the step (1), the weight ratio of the aging resistant agent to the copper propionate to the emulsifier to the surfactant to the water is 5-10: 3-5: 0.4-0.8: 0.2-0.6: 80-100.
Preferably, in the step (2), in the preparation of the precursor emulsion, the mass ratio of the emulsion to the calcium chloride solution is 1: 0.3-0.6.
Preferably, the spraying speed in the step (3) is 100-300mL/min, and the size of the sprayed liquid drop is 30-80 μm.
Preferably, in the preparation of the microcapsule aging resistant agent in the step (3), the mass ratio of the sodium carbonate solution to the calcium chloride solution is 0.5-1.4: 1.
preferably, in the preparation of the TPO waterproof roll raw material in the step (4), the mass ratio of the copolymerized TPO resin, the microcapsule aging resistant agent, the flame retardant, the dispersing agent and the filler is 100: 5-10: 10-30: 0.3-2: 20-30.
Preferably, the temperature of the melt plastification extrusion in the step (5) is 200-250 ℃.
In practical application, the TPO waterproof coiled material is easy to age under the influence of construction process and environment, and the ageing resistance effect is influenced by damage and consumption of the ageing resistance due to the fact that the powdery or granular ageing resistance is also easy to influence by severe environment and improper welding process by the aid of the method of adding the powdery or granular ageing resistance. The invention creatively microencapsulates the aging resistant agent to form a shell structure on the surface of the aging resistant agent, so that the aging resistant agent can be slowly released, the aging resistant agent can be protected, the uniform dispersion effect is achieved, and the aging resistance of the TPO waterproof coiled material can be obviously improved after the TPO waterproof coiled material is added.
The invention takes the aging resistant agent as a core and calcium carbonate as a shell structure to form the microcapsule aging resistant agent. The specific method comprises the following steps: wetting the anti-aging agent by using acetone, and then adding the anti-aging agent, an emulsifier, a surfactant and a calcium chloride solution into water in sequence to prepare a precursor emulsion, wherein the interfacial bonding property of the surface of the anti-aging agent is improved by the lubrication of the acetone, so that the subsequent reaction and generation of a core surface shell structure of the anti-aging agent are facilitated; the sodium carbonate solution is added into the precursor emulsion through an atomizing spray gun, and the sodium carbonate enters the precursor emulsion in uniform small drops by controlling the spraying speed and the size of atomized liquid drops, so that a uniform calcium carbonate coating layer, namely a shell structure of the microcapsule, is formed on the surface of the aging-resistant agent after the sodium carbonate reacts with calcium chloride. The affinity of the calcium carbonate and the resin is good, the rigidity, the toughness, the bending strength and the like of the material can be effectively increased or adjusted, the rheological property of a plastic processing system can be improved, the plasticizing temperature is reduced, the size stability, the heat resistance and the surface smoothness of the product are improved, and therefore, the calcium carbonate coating layer on the surface of the aging resistant agent can improve the strength and the heat resistance of the aging resistant agent. In the reaction process, an anionic surfactant in the precursor emulsion is combined with calcium ions in an ionic bond complexing mode, so that a large amount of calcium ions are enriched on the surface of emulsion liquid drops, calcium carbonate is promoted to form a shell structure on the surface of the emulsion liquid drops, and meanwhile, the calcium carbonate is used as the shell structure and is the same as TPO coiled material filler, and other performances of the TPO coiled material cannot be influenced after the calcium carbonate is added; in addition, the microencapsulated aging resistant agent has small size, can be uniformly dispersed in TPO resin, and can not generate microcapsule rupture during melt plasticizing extrusion, thereby effectively improving the aging resistance of the TPO waterproof coiled material.
The existing aging resistant agent is easy to damage in particle state when TPO coiled materials are subjected to melt plasticizing extrusion, is easy to consume under the influence of external severe environment, influences the aging resistance of the TPO coiled materials and limits the application of the TPO coiled materials. In view of the above, the invention provides an aging-resistant TPO building waterproof coiled material and a preparation method thereof, wherein an emulsifier and a surfactant are added into water, stirred and dispersed uniformly, the aging-resistant agent is ground and mixed uniformly, and a small amount of acetone is added dropwise for wetting, then the mixture is added into a mixed solution of the surfactant and the emulsifier, stirred and dispersed to obtain an emulsion; slowly dripping the calcium chloride solution into the emulsion, and continuously stirring to obtain stable precursor emulsion; slowly spraying a sodium carbonate solution into the precursor emulsion through an atomizing spray gun, so that the sodium carbonate enters the precursor emulsion in uniform small droplets, forming a uniform calcium carbonate coating layer on the surface of the anti-aging agent, continuously stirring after the dripping is finished, standing, centrifugally separating and drying to obtain the microcapsule anti-aging agent; adding the copolymerized TPO resin, the microcapsule anti-aging agent, the flame retardant, the dispersant and the filler into a high-speed stirrer, and uniformly mixing to obtain a TPO waterproof coiled material raw material; and conveying the TPO waterproof roll material layer raw material to a screw extruder for melting plasticization extrusion, conveying the material subjected to melting plasticization extrusion to a calender through a die head, and cooling, correcting, trimming, cutting and rolling to obtain the aging-resistant TPO building waterproof roll material. The microcapsule aging resistant agent with the aging resistant agent as the core and the calcium carbonate as the shell structure improves the strength and the heat resistance of the aging resistant agent, meanwhile, the microcapsule aging resistant agent can be uniformly dispersed into a TPO waterproof coiled material, the calcium carbonate shell structure cannot influence other properties of the coiled material, and the obtained waterproof coiled material has good mechanical property and stability and excellent aging resistance.
Compared with the prior art, the invention provides an aging-resistant TPO building waterproof coiled material and a preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. the microcapsule aging resistant agent with the aging resistant agent as the core and the calcium carbonate as the shell structure, which is prepared by the invention, improves the strength and the heat resistance of the aging resistant agent, and meanwhile, the microcapsule aging resistant agent can be uniformly dispersed into a TPO waterproof coiled material, the shell structure of the calcium carbonate does not influence other properties of the coiled material, and the obtained waterproof coiled material has good mechanical properties and stability and excellent aging resistance.
2. The preparation method is simple and controllable, the calcium carbonate coating formed on the surface of the aging resistant agent has good uniformity, the microencapsulated aging resistant agent has small size, can be uniformly dispersed in TPO resin, and can not generate microcapsule rupture in melt plasticizing extrusion and external severe environment, thereby improving the lasting aging resistance of the TPO waterproof coiled material.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding 0.6kg of Tween 80 emulsifier and 0.4kg of sodium dodecyl sulfate into 90kg of water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing uniformly 7.5kg of ageing resistant agent, wherein the ageing resistant agent is a Pasf 1010 antioxidant and a Pasf light stabilizer 2020 according to the mass ratio of 1: 1.5, dripping 4kg of acetone for wetting, then adding the mixture into the mixed solution, and uniformly dispersing at a stirring speed of 400r/min to obtain emulsion;
(2) slowly dripping 0.45kg of calcium chloride solution with the mass fraction of 15% into 1kg of emulsion, and continuously stirring for 2 hours to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution with the mass fraction of 15% into a precursor emulsion containing a calcium chloride solution through an atomizing spray gun, wherein the mass ratio of the sodium carbonate solution to the calcium chloride solution is 1: 1, spraying at the speed of 200mL/min, wherein the size of sprayed liquid drops is 55 microns, so that sodium carbonate enters a precursor emulsion in uniform small drops, a uniform calcium carbonate coating layer is formed on the surface of the anti-aging agent, then stirring is continued for 1h, standing is carried out for 6h, centrifugal separation is carried out, and drying is carried out in an oven at the temperature of 45 ℃ to obtain the microcapsule anti-aging agent;
(4) 100kg of polymer Engage8150 of ethylene and alpha-olefin produced by Dow company, 7.5kg of microcapsule anti-aging agent, 20kg of stearic acid surface modified magnesium hydroxide, 1.2kg of polyethylene wax and 25kg of light calcium carbonate with the fineness of 200 meshes are added into a high-speed stirrer and uniformly mixed to obtain TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material into a screw extruder, performing melt plasticizing extrusion at the temperature of 225 ℃, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then performing cooling, deviation correction, edge cutting, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Example 2
(1) Adding 0.5kg of Tween 80 emulsifier and 0.3kg of sodium dodecyl benzene sulfonate into 95kg of water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing uniformly 6kg of ageing resistant agent, wherein the ageing resistant agent is a Pasf 168 antioxidant and a Pasf light stabilizer 622SF according to the mass ratio of 1: 1.2, dripping 3.5kg of acetone for wetting, then adding the mixture into the mixed solution, and uniformly dispersing at a stirring speed of 350r/min to obtain emulsion;
(2) slowly dripping 0.4kg of calcium chloride solution with the mass fraction of 12% into 1kg of emulsion, and continuously stirring for 1.5h to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution with the mass fraction of 12% into the precursor emulsion containing the calcium chloride solution through an atomizing spray gun, wherein the mass ratio of the sodium carbonate solution to the calcium chloride solution is 0.7: 1, spraying at the speed of 150mL/min, wherein the size of a spray droplet is 40 μm, so that sodium carbonate enters a precursor emulsion in uniform small droplets, a uniform calcium carbonate coating layer is formed on the surface of the anti-aging agent, then stirring is continued for 1h, standing is carried out for 5.5h, centrifugal separation is carried out, and then drying is carried out in a 42 ℃ oven, so as to obtain the microcapsule anti-aging agent;
(4) 100kg of polymer Engage8150 of ethylene and alpha-olefin produced by Dow company, 6kg of microcapsule anti-aging agent, 15kg of stearic acid surface modified magnesium hydroxide, 0.8kg of polyethylene wax and 23kg of magnesium aluminum hydrotalcite with fineness being sieved by a 300-mesh sieve are added into a high-speed stirrer and are uniformly mixed to obtain TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material into a screw extruder, performing melt plasticizing extrusion at the temperature of 210 ℃, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then performing cooling, deviation correction, edge cutting, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Example 3
(1) Adding 0.7kg of Tween 80 emulsifier and 0.5kg of oleoyloxyethyl sodium sulfonate into 85kg of water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing uniformly 9kg of ageing resistant agent, wherein the ageing resistant agent is a Pasf 1010 antioxidant and a Pasf light stabilizer 622SF according to the mass ratio of 1: 1.8, dripping 4.5kg of acetone for wetting, then adding the mixture into the mixed solution, and uniformly dispersing at the stirring speed of 450r/min to obtain emulsion;
(2) slowly dripping 0.5kg of calcium chloride solution with the mass fraction of 18% into 1kg of emulsion, and continuously stirring for 2.5h to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution with the mass fraction of 18% into a precursor emulsion containing a calcium chloride solution through an atomizing spray gun, wherein the mass ratio of the sodium carbonate solution to the calcium chloride solution is 1.2: 1, spraying at a speed of 250mL/min, wherein the size of a spray droplet is 70 μm, so that sodium carbonate enters a precursor emulsion in uniform small droplets, a uniform calcium carbonate coating layer is formed on the surface of the anti-aging agent, then continuously stirring for 1.5h, standing for 6.5h, then performing centrifugal separation, and drying in an oven at 48 ℃ to obtain the microcapsule anti-aging agent;
(4) 100kg of polymer Engage8150 of ethylene and alpha-olefin produced by Dow company, 9kg of microcapsule anti-aging agent, 25kg of stearic acid surface modified magnesium hydroxide, 1.6kg of polyethylene wax and 26kg of light calcium carbonate which is finely sieved by a 200-mesh sieve are added into a high-speed stirrer and are uniformly mixed to obtain TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material into a screw extruder, performing melt plasticizing extrusion at the temperature of 240 ℃, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then performing cooling, deviation correction, edge cutting, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Example 4
(1) Adding 0.4kg of Tween 20 emulsifier and 0.2kg of sodium dodecyl sulfate into 100kg of water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing uniformly 5kg of ageing resistant agent, wherein the ageing resistant agent is a Pasf 168 antioxidant and a Pasf light stabilizer 2020 according to the mass ratio of 1: 1, dripping 3kg of acetone for wetting, then adding the mixture into the mixed solution, and uniformly dispersing at a stirring speed of 300r/min to obtain emulsion;
(2) slowly dripping 0.3kg of calcium chloride solution with the mass fraction of 10% into 1kg of emulsion, and continuously stirring for 1h to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution with the mass fraction of 10% into the precursor emulsion containing the calcium chloride solution through an atomizing spray gun, wherein the mass ratio of the sodium carbonate solution to the calcium chloride solution is 0.5: 1, spraying at a speed of 100mL/min, wherein the size of a spray droplet is 30 mu m, so that sodium carbonate enters a precursor emulsion in uniform small droplets, a uniform calcium carbonate coating layer is formed on the surface of the anti-aging agent, then continuously stirring for 0.5h, standing for 5h, performing centrifugal separation, and drying in an oven at the temperature of 40 ℃ to obtain the microcapsule anti-aging agent;
(4) 100kg of polymer Engage8150 of ethylene and alpha-olefin produced by Dow company, 5kg of microcapsule anti-aging agent, 10kg of stearic acid surface modified magnesium hydroxide, 0.3kg of polyethylene wax and 20kg of magnesium aluminum hydrotalcite which is finely sieved by a 200-mesh sieve are added into a high-speed stirrer and are uniformly mixed to obtain TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material into a screw extruder, performing melt plasticizing extrusion at the temperature of 200 ℃, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then performing cooling, deviation correction, edge cutting, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Example 5
(1) Adding 0.8kg of Tween 80 and 0.6kg of sodium dodecyl benzene sulfonate into 100kg of water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing uniformly 10kg of an aging resistant agent, wherein the aging resistant agent is a Pasf 168 antioxidant and a Pasf light stabilizer 622SF according to the mass ratio of 1: 2, dripping 5kg of acetone into the mixture for wetting, then adding the mixture into the mixed solution, and uniformly dispersing the mixture at a stirring speed of 500r/min to obtain emulsion;
(2) slowly dripping 0.6kg of calcium chloride solution with the mass fraction of 20% into 1kg of emulsion, and continuously stirring for 3 hours to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution with the mass fraction of 20% into the precursor emulsion containing the calcium chloride solution through an atomizing spray gun, wherein the mass ratio of the sodium carbonate solution to the calcium chloride solution is 1.4: 1, spraying at the speed of 300mL/min, wherein the size of a spray droplet is 80 μm, so that sodium carbonate enters a precursor emulsion in uniform small droplets, a uniform calcium carbonate coating layer is formed on the surface of the anti-aging agent, then continuously stirring for 2h, standing for 7h, performing centrifugal separation, and drying in an oven at the temperature of 45 ℃ to obtain the microcapsule anti-aging agent;
(4) 100kg of polymer Engage8150 of ethylene and alpha-olefin produced by Dow company, 10kg of microcapsule anti-aging agent, 30kg of stearic acid surface modified magnesium hydroxide, 2kg of polyethylene wax and 30kg of light calcium carbonate with fineness being screened by a 300-mesh sieve are added into a high-speed stirrer and are uniformly mixed to obtain TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material into a screw extruder, performing melt plasticizing extrusion at the temperature of 250 ℃, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then performing cooling, deviation correction, edge cutting, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
Comparative example 1
Comparative example 1 compared with example 1, the weathering agent was not microencapsulated, and the rest was completely identical to example 1.
The test method comprises the following steps:
and (3) performance testing: the test method refers to the standards of Thermoplastic Polyolefin (TPO) waterproof coiled material (GB 27789-:
(1) and (3) testing the thickness of the coiled material:
the size of the test piece is set as 10000mm of the area of a square test piece2Uniformly cutting 5 test pieces of the waterproof coiled material prepared by the embodiment and the comparative example in the width direction of the coiled material, wherein the distance between the test piece at the outermost end and the edge of the coiled material is 100 mm; then placing the test piece for 20h under the conditions that the temperature is 23 ℃ and the relative humidity is 50%, then testing at 23 ℃, and measuring the thickness of each test piece by a mechanical measurement method;
(2) tensile Property test
Cutting two 150 multiplied by 50mm test pieces from the waterproof roll prepared in the embodiment and the comparative example, tightly clamping the test pieces in a clamp of a tensile testing machine, enabling the center line of the test piece in the length direction to be in the same line with the center of the clamp of the testing machine, testing at the temperature of 23 ℃, continuously recording the tensile force and the separation distance between corresponding clamps until the test pieces break, and calculating the maximum tensile force and the elongation;
(3) heat treatment dimensional Change Rate test
Three 250X 250mm square test pieces prepared in the examples and the comparative examples are respectively placed in a blast oven at 80 ℃ without overlapping, then the temperature is kept for 24 hours, the test pieces are taken out and placed in an environment with the temperature of 23 ℃ and the humidity of 50 percent for 24 hours, the length of the test pieces is measured, and the heat treatment length change rate is calculated according to the ratio of the length difference value before and after the experiment to the initial value;
(4) thermal aging test
Two test pieces of 300X 150mm size were cut out from each of the examples and comparative examples, and then placed in a hot air test chamber at 115 ℃ for 672 hours, and then taken out, and after the test pieces were placed in an environment of 23 ℃ and 50% humidity for 24 hours, the appearance was inspected, and the tensile properties were measured.
(5) Artificial climate accelerated aging test
Cutting two test pieces with the specification of 300 multiplied by 150mm respectively according to the embodiment and the comparative example of the invention, then placing the test pieces in an artificial climate accelerated aging test box for xenon arc lamp test, wherein the irradiation time is 2500h, then taking out the test pieces, placing the test pieces in an environment with the temperature of 23 ℃ and the humidity of 50% for 24h, and then measuring the tensile property;
the test results are shown in table 1.
Table 1:
as can be seen from table 1, the aging resistance of the aging-resistant TPO building waterproof roll prepared in the embodiment of the present invention is excellent, the retention rate and the tensile strength retention rate of the waterproof roll in the embodiment after the aging test are both higher than those of the comparative example, and the yellow index difference is lower than that of the waterproof roll in the comparative example, so that the waterproof roll produced by the present invention has excellent aging resistance and has a more durable aging resistance in a severe environment.
Claims (10)
1. An aging-resistant TPO building waterproof coiled material is characterized in that an aging-resistant agent is wetted by acetone and then uniformly dispersed with an emulsifier, a surfactant and water to obtain emulsion, then a calcium chloride solution is slowly added to obtain a precursor emulsion, a sodium carbonate solution is sprayed into the precursor emulsion, the microcapsule aging-resistant agent is obtained through stirring, standing, centrifugal separation and drying, then the microcapsule aging-resistant agent is uniformly mixed with a copolymer TPO resin, a flame retardant, a dispersing agent and a filler to obtain a TPO waterproof coiled material raw material, and then the TPO waterproof coiled material is prepared through melt plasticizing extrusion, calendaring, cooling, deviation correction, edge cutting, cutting and rolling.
2. The aging-resistant TPO building waterproofing membrane of claim 1, characterized in that:
the anti-aging agent is an antioxidant and a light stabilizer in a mass ratio of 1: 1-2, the antioxidant is one or a combination of two of basf 1010 and basf 168, and the light stabilizer is one or a combination of two of basf 2020 and 622 SF;
the emulsifier is one of tween 80 and tween 20;
the surfactant is one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium oleoyloxy ethanesulfonate;
the copolymerized TPO resin is Engage8150 produced by Dow company;
the flame retardant is magnesium hydroxide modified by stearic acid surface;
the dispersing agent is polyethylene wax;
the filler is one of light calcium carbonate and magnesium aluminum hydrotalcite, and the fineness of the filler is 200-300-mesh sieve.
3. The aging-resistant TPO building waterproofing membrane according to claim 1,
the mass fraction of the calcium chloride solution is 10-20%;
the mass fraction of the sodium carbonate solution is 10-20%.
4. The method for preparing an aging-resistant TPO building waterproofing membrane as claimed in any of claims 1 to 3, wherein the specific preparation method is as follows:
(1) adding an emulsifier and a surfactant into water, stirring and dispersing uniformly to obtain a mixed solution, then grinding and mixing the aging-resistant agent uniformly, dripping a small amount of acetone for wetting, then adding the acetone into the mixed solution, and dispersing uniformly at a stirring speed of 300-500r/min to obtain an emulsion;
(2) slowly dripping the calcium chloride solution into the emulsion, and continuously stirring for 1-3h to obtain stable precursor emulsion;
(3) slowly spraying a sodium carbonate solution into a precursor emulsion containing a calcium chloride solution through an atomizing spray gun, so that the sodium carbonate enters the precursor emulsion in uniform small droplets, forming a uniform calcium carbonate coating layer on the surface of the anti-aging agent, continuously stirring for 0.5-2h, standing for 5-7h, performing centrifugal separation, and drying in an oven at the temperature of 40-50 ℃ to obtain the microcapsule anti-aging agent;
(4) adding the copolymerized TPO resin, the microcapsule aging resistant agent, the flame retardant, the dispersing agent and the filler into a high-speed stirrer, and uniformly mixing to obtain a TPO waterproof coiled material raw material;
(5) conveying the TPO waterproof coiled material raw material to a screw extruder for melt plasticizing extrusion, conveying the material subjected to melt plasticizing extrusion to a calender through a die head, and then cooling, correcting, trimming, cutting and rolling to obtain the aging-resistant TPO building waterproof coiled material.
5. The method for preparing an aging-resistant TPO building waterproof coiled material as claimed in claim 4, wherein in the emulsion preparation in step (1), the weight ratio of aging-resistant agent, copper propionate, emulsifier, surfactant and water is 5-10: 3-5: 0.4-0.8: 0.2-0.6: 80-100.
6. The method for preparing an aging-resistant TPO building waterproofing membrane according to claim 4, wherein in the step (2), the mass ratio of the emulsion to the calcium chloride solution is 1: 0.3-0.6.
7. The method for preparing an aging-resistant TPO building waterproofing membrane according to claim 4, wherein the spraying speed in step (3) is 100-300mL/min, and the spray droplet size is 30-80 μm.
8. The method for preparing an aging-resistant TPO building waterproof coiled material as claimed in claim 4, wherein in the preparation of the microcapsule aging-resistant agent in step (3), the mass ratio of sodium carbonate solution to calcium chloride solution is 0.5-1.4: 1.
9. the method for preparing an aging-resistant TPO building waterproof roll according to claim 4, wherein in the preparation of the TPO waterproof roll raw material in the step (4), the mass ratio of the copolymerized TPO resin, the microcapsule aging-resistant agent, the flame retardant, the dispersant and the filler is 100: 5-10: 10-30: 0.3-2: 20-30.
10. The method for preparing an aging-resistant TPO building waterproofing membrane according to claim 4, wherein the temperature of the melt plastication extrusion in step (5) is 200-250 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708181A (en) * | 2020-12-26 | 2021-04-27 | 安徽酉阳防水科技有限公司 | Nano modified weather-resistant TPO waterproof coiled material |
| CN115960469A (en) * | 2022-12-13 | 2023-04-14 | 赛轮集团股份有限公司 | Preparation method and application of protective wax slow-release microcapsule |
| CN116041865A (en) * | 2023-01-03 | 2023-05-02 | 辽宁威科特瑞阻燃材料科技有限公司 | TPO waterproofing membrane that is difficult for ageing |
-
2020
- 2020-07-08 CN CN202010650821.5A patent/CN111875870A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708181A (en) * | 2020-12-26 | 2021-04-27 | 安徽酉阳防水科技有限公司 | Nano modified weather-resistant TPO waterproof coiled material |
| CN115960469A (en) * | 2022-12-13 | 2023-04-14 | 赛轮集团股份有限公司 | Preparation method and application of protective wax slow-release microcapsule |
| CN115960469B (en) * | 2022-12-13 | 2024-03-15 | 赛轮集团股份有限公司 | Preparation method and application of protective wax slow-release microcapsule |
| CN116041865A (en) * | 2023-01-03 | 2023-05-02 | 辽宁威科特瑞阻燃材料科技有限公司 | TPO waterproofing membrane that is difficult for ageing |
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