CN111995946A - Polyurethane root-resistant waterproof coating and preparation method thereof - Google Patents
Polyurethane root-resistant waterproof coating and preparation method thereof Download PDFInfo
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- CN111995946A CN111995946A CN202010869934.4A CN202010869934A CN111995946A CN 111995946 A CN111995946 A CN 111995946A CN 202010869934 A CN202010869934 A CN 202010869934A CN 111995946 A CN111995946 A CN 111995946A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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Abstract
The invention relates to the field of a root-resistant coating, and discloses a polyurethane root-resistant waterproof coating and a preparation method thereof. The preparation process comprises the following steps: (1) adding thermoplastic polyurethane elastomer rubber (TPU) and nano copper powder into a screw extruder to prepare TPU-coated nano copper powder; (2) grinding the TPU-coated nano copper powder to prepare the TPU-coated nano copper powder filler; (3) adding polyether polyol, TPU coated copper nanoparticle filler, pigment filler, plasticizer and other auxiliaries into a reaction kettle in sequence, heating and carrying out vacuum dehydration to obtain a uniformly mixed raw material; (4) cooling the uniformly mixed raw materials, and adding isocyanate to react to prepare a mixture A; (5) and adding a solvent and a latent curing agent into the mixture A, stirring, and discharging to obtain the single-component polyurethane root-blocking waterproof coating. The waterproof coating prepared by the invention has excellent root resistance, waterproof performance and root puncture resistance, is low in cost, has no harm to plants, is simple in production process, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of a root-resistant coating, and discloses a polyurethane root-resistant waterproof coating and a preparation method thereof.
Background
With the gradual improvement of environmental awareness of people, greening and planting projects become the main content of urban construction, and the buildings are the largest consumers of natural resources in society, so people usually cover landscapes such as green vegetation, rockery, pool and the like on the roof, the roof and the roof of the basement of the building, and create an ecological system which is pleasing and beautifies the environment. The planted roof is an effective way for improving the urban greening coverage rate, slowing down the heat island effect, reducing the atmospheric pollution, saving the energy, intercepting the rainwater, improving the ecological environment and beautifying the urban landscape.
As is well known, the building greening generally comprises planted plants, a waterproof root-blocking layer, a water drainage and storage device, a heat-preservation and heat-insulation layer and the like, wherein the waterproof root-blocking layer is particularly important. Any greening plant works are faced with the problem of water leakage prevention because the planted plants have developed root systems that can penetrate the roof structure layer to cause severe water leakage. Therefore, when the plant roots planted on the roof have strong penetrating ability, they can penetrate the roof structure layer to cause serious water leakage. At present, a planted roof usually adopts waterproof coiled materials, polyurea spraying, waterproof coating brushing and the like to resist roots and prevent water, so that the purpose of preventing roots in the planted roof is achieved.
Among the root-resistant waterproof coatings, the polyurethane waterproof coating belongs to a chemical reaction type waterproof coating, is a rubber-like high-elasticity coating after being cured, is seamless as a whole, and is suitable for root resistance and water resistance of planted roofs. Polyurethane waterproof coatings are classified into two main categories, single-component and multi-component, according to their composition and curing mechanism. The multi-component polyurethane waterproof coating needs to be proportioned according to a certain proportion and mechanically stirred during field construction, inaccurate proportioning is easily caused by field construction proportioning, bubbles are easily introduced in the mechanical stirring process, the construction quality is influenced, and even waterproof quality accidents are caused; the single-component polyurethane waterproof coating has single component, can be used immediately after being opened, does not need stirring, has reliable construction and can be widely applied. At present, the root penetration resistance effect is mainly achieved by adding a chemical root-resisting agent or nano copper powder in the polyurethane waterproof coating.
Chinese patent application No. 201910614768.0 discloses a reactive root-resistant polyurethane waterproof coating root-resistant agent and a preparation method thereof, wherein the molecular structure of the root-resistant agent contains a root-resistant active group and one or two hydroxyl groups capable of chemically reacting with isocyanate which is a main component group in a polyurethane coating. Hydroxyl introduces active groups with root-resistant effect into the waterproof coating in a form of end capping or chain extension, so as to become a real reaction type root-resistant polyurethane waterproof coating root-resistant agent. The invention mainly uses chlorine-containing root-stopping groups as root-stopping agents, but chlorine-containing organic matters are toxic to plants generally, so that the plants can die when the roots are stopped.
The Chinese patent application No. 201811119655.5 discloses a high-molecular environment-friendly polyurethane root-resistant puncture-resistant waterproof coating for a planted roof, which comprises the following components in parts by weight: 15-20 parts of polyether 2000N, 5-10 parts of polyether 330N, 4-6 parts of MDI, 0.06-0.1 part of catalyst, 1-1.5 parts of latent curing agent, 0.5-1.5 parts of root inhibitor, 0.2-0.5 part of dispersant, 0.2-0.5 part of defoaming agent, 0.2-0.5 part of antioxidant, 45-55 parts of filler and 1-2 parts of anti-settling agent. The invention mainly uses the chemical root-resisting agent as the root-resisting material, and the root-resisting material is an imported material and is expensive, so that the product cost is increased.
Chinese patent application No. 201710448039.3 discloses a root-puncture-resistant water-based waterproof paint which is prepared from liquid materials and powder materials; the liquid material comprises the following components in percentage by weight: 85-95% of VAE emulsion, 1-3% of defoaming agent, 0-0.3% of mildew preventive and 5-15% of water; the formula of the powder comprises the following components in percentage by weight: 40-60% of white cement, 20-40% of barium sulfate, 10-20% of quartz sand, 1-3% of a water reducing agent, 1-15% of copper sulfate, 1-15% of nano copper powder, 1-15% of nano zinc oxide and 0.1-1% of a chemical root-resisting agent. The nano copper powder in the invention has poor dispersibility, thereby influencing the root-resisting effect of the coating.
According to the polyurethane waterproof coating for preventing the roots of the roof in the existing scheme, the chemical root-preventing agent with low price can damage the plants, the chemical root-preventing agent which is harmless to the plants is high in cost, the coating cost is greatly increased after the chemical root-preventing agent is added, and in addition, the nano copper powder is extremely easy to oxidize and agglomerate, so that the dispersibility is obviously reduced when the nano copper powder is directly added into a coating system, and the root-preventing effect is influenced.
Disclosure of Invention
The chemical root-blocking agent added into the widely-applied root-blocking waterproof coating at present can have adverse effects on plant growth, the cost of the harmless chemical root-blocking agent is high, and in addition, the problems of easiness in oxidation and poor dispersibility exist when the nano copper powder is added.
The invention solves the problems through the following technical scheme:
a preparation method of polyurethane root-resistant waterproof paint comprises the following specific steps:
(1) firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the raw materials comprise, by weight, 100-120 parts of thermoplastic polyurethane elastomer rubber and 10-15 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro powder mill for grinding for 2-3 h, then sieving with a 1250-mesh sieve, and collecting to prepare the TPU coated nano copper powder filler;
(3) adding polyether polyol into a closed reaction kettle, heating to 70-90 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding the pigment filler, the plasticizer and other auxiliaries, continuously heating to 100-130 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the raw materials comprise, by weight, 20-40 parts of polyether polyol, 5-10 parts of TPU coated nano copper powder filler, 3-5 parts of pigment filler, 5-10 parts of plasticizer and 0.3-0.8 part of other additives;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 30-40 ℃, adding isocyanate, stirring and reacting for 1-2 hours, heating to 60-100 ℃, and continuously stirring and reacting for 3-5 hours to obtain a mixture A;
(5) cooling the mixture A obtained in the step (4) to 30-50 ℃, adding a solvent and a latent curing agent, continuously stirring for 1-2 hours, cooling to 30-40 ℃, introducing an inert gas for protection for 50-100 min, and discharging to obtain a single-component polyurethane waterproof coating; the raw material mixture ratio is, by weight, 10-15 parts of a solvent, 0.4-1 part of a latent curing agent and 30-80 parts of a mixture A.
The thermoplastic polyurethane elastomer (TPU) is an elastomer which can be plasticized by heating and can be dissolved by a solvent, and has excellent comprehensive properties of high strength, high toughness, wear resistance, oil resistance and the like and good processing performance. According to the invention, the thermoplastic polyurethane elastomer rubber is used for coating the nano copper powder, so that the excellent characteristics of the thermoplastic polyurethane elastomer rubber can be effectively exerted, the polyurethane elastomer and the polyurethane prepolymer have the same chain segment and group, and in the preparation of the polyurethane waterproof coating in the subsequent preparation process, the good compatibility of the polyurethane elastomer and the polyurethane prepolymer ensures that the TPU coated copper powder does not separate, so that the waterproof performance and the root penetration resistance of the polyurethane waterproof coating can be improved, and meanwhile, the nano copper powder can be uniformly dispersed in the coating, and a good root blocking effect can be exerted. Preferably, the thermoplastic polyurethane elastomer rubber in the step (1) is a Coresian injection molding grade TPU; as a further preferred aspect of the present invention, the thermoplastic polyurethane elastomer rubber is TPU 9852D.
Preferably, the screw extruder in the step (1) is one of a single screw extruder, a double screw extruder and a three screw extruder, the length-diameter ratio of the screws is 20-30, and the rotating speed is 100-120 r/min; the temperature of each heating section of the screw extruder is 150-160 ℃ in the feeding section, 180-210 ℃ in the melting section and 170-180 ℃ in the homogenizing section.
The nanometer copper powder has the characteristic of avoiding the root system of the plant, and can not cause damage to the plant when being used as a root blocking filler with excellent performance. In the present invention, the particle size of the copper nanoparticles in step (1) is preferably 20 to 100 nm. The feeding speed of the nano copper powder must be effectively controlled in the feeding process, so that the uniform dispersion of the nano copper powder is realized, and as a further optimization of the invention, the feeding speed of the nano copper powder in a screw extruder is 50-200 g/min.
Preferably, the tricyclic ring fine mill in the step (2) is ZYM tricyclic ring fine mill of ZYM, the specific model can be ZYM80, the rotating speed of a main shaft is 235-240 r/min, the number of grinding rings is 3, and the number of grinding rolls is 20.
The conventional method for synthesizing the water-based reactive polyurethane by reacting the polyether polyol with the bifunctional isocyanate has the advantages of easily controlled reaction process and good product performance, and is a good choice for the preparation process of the polyurethane waterproof coating.
Preferably, in the step (3), the polyether polyol is at least one of PPG polyether polyol, POP polymer polyether polyol and polytetrahydrofuran polyether polyol, and has a molecular weight of 500-5000.
Preferably, the pigment and filler in step (3) is at least one of carbon black, titanium dioxide, iron oxide yellow, kaolin, wollastonite and talcum powder.
Preferably, the plasticizer in step (3) is one of dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, chlorinated paraffin and citric acid ester.
Preferably, the other auxiliary agents in the step (3) are a mixture prepared from a defoaming agent, a dispersing agent and an antioxidant according to a mass ratio of 1: 0.5-1: 0.8-2.
As a further preferable mode of the invention, the defoaming agent is BYK-064, the dispersing agent is DY-9006, and the antioxidant is T-501.
Preferably, the vacuum degree of the vacuum dehydration in the step (3) is-0.09 to-0.1 MPa, and the time is 2 to 3 hours.
In the present invention, the isocyanate in the step (4) is preferably one of 1, 6-hexamethylene diisocyanate and isophorone diisocyanate.
In a further preferred embodiment of the present invention, the amount of the isocyanate added is 0.8 to 1.2 times the weight of the polyether polyol.
Preferably, the solvent in step (5) is 150# solvent oil.
As a preferred aspect of the present invention, the latent curing agent of step (5) is one of 2-isopropyl-N-hydroxyethyl-oxazolidine, 2-isopropyl oxazolidine, and 2, 2-dihydro oxazolidine.
Preferably, the inert gas in step (5) is one of helium, neon and argon.
The polyurethane root-blocking waterproof coating prepared by the method has the advantages of good root-blocking performance, no harm to plants, simple production process, low price and suitability for large-scale production.
The invention provides a polyurethane root-resistant waterproof coating and a preparation method thereof.A thermoplastic polyurethane elastomer (TPU) is added into a screw extruder, the temperature of each heating section of a screw and the rotating speed parameter of the screw are set, the whole process is carried out under the protection of nitrogen, after the polyurethane elastomer rubber is molten, nano copper powder is slowly added under the protection of nitrogen at a second feeding port, and after uniform mixing, the mixture is extruded and granulated to obtain TPU-coated nano copper powder; adding the obtained TPU-coated nano copper powder into a three-ring micro powder mill for grinding, and then sieving to obtain TPU-coated nano copper powder filler; adding polyether polyol into a closed reaction kettle, heating, then continuously adding the obtained TPU coated nano copper powder filler, stirring and mixing uniformly, continuously adding pigment filler, plasticizer and other auxiliaries, heating continuously, and dehydrating under a vacuum condition to obtain a uniformly mixed raw material; cooling the uniformly mixed raw materials, adding isocyanate, stirring for reaction, and then heating until the stirring reaction is continued; and cooling, adding the solvent and the latent curing agent, continuing stirring, cooling, introducing inert gas for protection, and discharging.
The invention provides a polyurethane root-resistant waterproof coating and a preparation method thereof, and compared with the prior art, the polyurethane root-resistant waterproof coating has the outstanding characteristics and excellent effects that:
1. provides a method for preparing polyurethane root-resistant waterproof coating by coating nano copper powder on a thermoplastic polyurethane elastomer.
2. The nano copper powder and polyurethane are mixed, granulated and ground to be used as a filler, so that the nano copper powder is prevented from being added into a coating system to be agglomerated, the nano copper powder has good dispersibility in the coating, and the good root resistance of the nano copper powder is exerted.
3. The polyurethane elasticity and the polyurethane prepolymer used in the invention have the same chain segment and group, so that the polyurethane has good compatibility, and the TPU coated copper powder can not be separated, thereby improving the waterproof performance and the root penetration resistance of the polyurethane waterproof coating.
4. The method of the invention avoids using expensive chemical root-resisting agent, so that the cost of the coating is reduced, and meanwhile, the coating has no harm to plants.
Drawings
FIG. 1 is a process flow chart of preparing TPU coated copper nanoparticles in preparing polyurethane root-blocking waterproof coating according to the present invention; wherein: 1 is a screw extruder, 2 is TPU, 3 is nano copper powder, and 4 is a three-ring micro-mill.
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) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a single screw extruder, the length-diameter ratio of the screw is 30, and the rotating speed is 120 r/min; the temperature of each heating interval of the screw extruder is 155 ℃ in a feeding section, 190 ℃ in a melting section and 175 ℃ in a homogenizing section; the particle size of the nano copper powder is 70nm, and the feeding speed of the nano copper powder in a screw extruder is 130 g/min;
the raw materials comprise 108 parts by weight of thermoplastic polyurethane elastomer rubber and 15 parts by weight of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro powder mill for grinding for 2.5h, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer in Zoya, the rotating speed of the main shaft is 238r/min, the number of grinding rings is 3, and the number of grinding rollers is 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 78 ℃, adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding pigment filler, plasticizer and other auxiliaries, continuously heating to 108 ℃, and performing vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is PPG polyether polyol; the pigment and the filler are carbon black; the plasticizer is dioctyl phthalate; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to a mass ratio of 1:0.7: 1.3; the vacuum degree of vacuum dehydration is-0.095 MPa, and the time is 2.5 h;
the raw materials comprise, by weight, 28 parts of polyether polyol, 5 parts of TPU coated nano copper powder filler, 5 parts of pigment filler, 7 parts of plasticizer and 0.5 part of other additives;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 36 ℃, adding isocyanate, stirring and reacting for 1.5h, heating to 90 ℃, and continuously stirring and reacting for 4.5h to obtain a mixture A; the isocyanate is 1, 6-hexamethylene diisocyanate, and the adding amount of the isocyanate is 1.1 times of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 38 ℃, adding a solvent and a latent curing agent, continuously stirring for 1.5h, cooling to 36 ℃, introducing inert gas for protection for 70min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2-isopropyl-N-hydroxyethyl-oxazolidine; the inert gas is helium;
the raw material mixture ratio is, by weight, mixture A60 parts, solvent 13 parts, latent curing agent 0.6 parts.
The polyurethane root-blocking waterproof coating prepared in example 1 has the root-blocking performance shown in table 1.
Example 2
(1) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a double-screw extruder, the length-diameter ratio of a screw is 30, and the rotating speed is 120 r/min; the temperature of each heating interval of the screw extruder is 150 ℃ in a feeding section, 185 ℃ in a melting section and 170 ℃ in a homogenizing section; the particle size of the nano copper powder is 30nm, and the feeding speed of the nano copper powder in a screw extruder is 80 g/min;
the raw materials comprise, by weight, 115 parts of thermoplastic polyurethane elastomer rubber and 15 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro-powder mill for grinding for 2 hours, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer of ZYM, with main shaft rotation speed of 235r/min, grinding rings number of 3, and grinding rollers number of 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 75 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding pigment filler, plasticizer and other auxiliaries, continuously heating to 110 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is POP polymer polyether polyol; the pigment and filler is titanium dioxide; the plasticizer is dibutyl phthalate; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to the mass ratio of 1:0.6: 1; the vacuum degree of vacuum dehydration is-0.09 MPa, and the time is 3 h;
the raw materials comprise, by weight, 35 parts of polyether polyol, 5 parts of TPU coated nano copper powder filler, 5 parts of pigment filler, 6 parts of plasticizer and 0.4 part of other additives;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 32 ℃, adding isocyanate, stirring and reacting for 2 hours, heating to 70 ℃, and continuously stirring and reacting for 4.5 hours to obtain a mixture A; the isocyanate is isophorone diisocyanate, and the adding amount of the isocyanate is 0.9 times of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 35 ℃, adding a solvent and a latent curing agent, continuously stirring for 2 hours, cooling to 32 ℃, introducing inert gas for protection for 90min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2-isopropyl oxazolidine; the inert gas is neon;
the raw material mixture ratio is, by weight, mixture A70 parts, solvent 11 parts, latent curing agent 0.5 parts.
The polyurethane root-blocking waterproof coating prepared in example 2 has the root-blocking performance shown in table 1.
Example 3
(1) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a three-screw extruder, the length-diameter ratio of screws is 30, and the rotating speed is 100 r/min; the temperature of each heating interval of the screw extruder is 160 ℃ in a feeding section, 205 ℃ in a melting section and 180 ℃ in a homogenizing section; the particle size of the nano copper powder is 80nm, and the feeding speed of the nano copper powder in a screw extruder is 180 g/min;
the raw materials comprise, by weight, 105 parts of thermoplastic polyurethane elastomer rubber and 15 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro-powder mill for grinding for 3 hours, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer in ZYM, with spindle rotation speed of 240r/min, grinding rings number of 3, and grinding rollers number of 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 85 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding the pigment filler, the plasticizer and other auxiliaries, continuously heating to 125 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is polytetrahydrofuran polyether polyol; the pigment and filler is iron yellow; the plasticizer is diisononyl phthalate; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to a mass ratio of 1:0.9: 1.5; the vacuum degree of vacuum dehydration is-0.1 MPa, and the time is 2 h;
the raw materials comprise, by weight, 25 parts of polyether polyol, 8 parts of TPU coated nano copper powder filler, 3 parts of pigment filler, 9 parts of plasticizer and 0.7 part of other auxiliary agents;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 38 ℃, adding isocyanate, stirring and reacting for 2 hours, heating to 90 ℃, and continuously stirring and reacting for 3 hours to obtain a mixture A; the isocyanate is 1, 6-hexamethylene diisocyanate, and the adding amount of the isocyanate is 1.1 times of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 45 ℃, adding a solvent and a latent curing agent, continuously stirring for 1h, cooling to 38 ℃, introducing inert gas for protection for 90min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2, 2-dihydrooxazolidine; the inert gas is argon;
the raw material mixture ratio is, by weight, mixture A40 parts, solvent 14 parts, latent curing agent 0.8 parts.
The polyurethane root-blocking waterproof coating prepared in example 3 has the root-blocking performance shown in table 1.
Example 4
(1) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a single screw extruder, the length-diameter ratio of the screw is 30, and the rotating speed is 120 r/min; the temperature of each heating interval of the screw extruder is 150 ℃ in a feeding section, 180 ℃ in a melting section and 170 ℃ in a homogenizing section; the particle size of the nano copper powder is 20nm, and the feeding speed of the nano copper powder in a screw extruder is 50 g/min;
the raw materials comprise, by weight, 120 parts of thermoplastic polyurethane elastomer rubber and 15 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro-powder mill for grinding for 2 hours, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer of ZYM, with main shaft rotation speed of 235r/min, grinding rings number of 3, and grinding rollers number of 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 70 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding the pigment filler, the plasticizer and other auxiliaries, continuously heating to 100 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is PPG polyether polyol; the pigment and filler is kaolin; the plasticizer is chlorinated paraffin; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to a mass ratio of 1:0.5: 0.8; the vacuum degree of vacuum dehydration is-0.09 Pa, and the time is 3 h;
the raw materials comprise, by weight, 40 parts of polyether polyol, 5 parts of TPU coated nano copper powder filler, 3 parts of pigment filler, 5 parts of plasticizer and 0.3 part of other auxiliary agents;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 30 ℃, adding isocyanate, stirring and reacting for 2 hours, heating to 60 ℃, and continuously stirring and reacting for 5 hours to obtain a mixture A; the isocyanate is isophorone diisocyanate, and the adding amount of the isocyanate is 0.8 times of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 30 ℃, adding a solvent and a latent curing agent, continuously stirring for 2 hours, cooling to 30 ℃, introducing inert gas for protection for 100min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2-isopropyl-N-hydroxyethyl-oxazolidine; the inert gas is helium;
the raw material mixture ratio is, by weight, mixture A80 parts, solvent 10 parts, latent curing agent 0.4 parts.
The polyurethane root-blocking waterproof coating prepared in example 4 has the root-blocking performance shown in table 1.
Example 5
(1) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a double-screw extruder, the length-diameter ratio of a screw is 30, and the rotating speed is 100 r/min; the temperature of each heating interval of the screw extruder is 160 ℃ in a feeding section, 210 ℃ in a melting section and 180 ℃ in a homogenizing section; the particle size of the nano copper powder is 100nm, and the feeding speed of the nano copper powder in a screw extruder is 200 g/min;
the raw materials comprise 100 parts by weight of thermoplastic polyurethane elastomer rubber and 15 parts by weight of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro-powder mill for grinding for 3 hours, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer in ZYM, with spindle rotation speed of 240r/min, grinding rings number of 3, and grinding rollers number of 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 90 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding pigment filler, plasticizer and other auxiliaries, continuously heating to 130 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is POP polymer polyether polyol; the pigment and the filler are wollastonite; the plasticizer is citric acid ester; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to a mass ratio of 1: 1: 2; the vacuum degree of vacuum dehydration is-0.1 MPa, and the time is 2 h;
the raw materials comprise, by weight, 20 parts of polyether polyol, 5 parts of TPU coated nano copper powder filler, 4 parts of pigment filler, 10 parts of plasticizer and 0.8 part of other auxiliary agents;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 40 ℃, adding isocyanate, stirring and reacting for 1h, heating to 100 ℃, and continuously stirring and reacting for 3h to obtain a mixture A; the isocyanate is 1, 6-hexamethylene diisocyanate, and the adding amount of the isocyanate is 1.2 times of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 50 ℃, adding a solvent and a latent curing agent, continuously stirring for 1h, cooling to 40 ℃, introducing inert gas for protection for 100min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2-isopropyl oxazolidine; the inert gas is neon;
the raw material mixture ratio is, by weight, mixture A30 parts, solvent 15 parts, latent curing agent 1 part.
The polyurethane root-blocking waterproof coating prepared in example 5 has the root-blocking performance shown in table 1.
Example 6
(1) Firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the thermoplastic polyurethane elastomer rubber is Coresi injection molding grade TPU 9852D; the screw extruder is a three-screw extruder, the length-diameter ratio of screws is 30, and the rotating speed is 100 r/min; the temperature of each heating interval of the screw extruder is 155 ℃ in a feeding section, 195 ℃ in a melting section and 175 ℃ in a homogenizing section; the particle size of the nano copper powder is 60nm, and the feeding speed of the nano copper powder in a screw extruder is 140 g/min;
the raw materials comprise, by weight, 110 parts of thermoplastic polyurethane elastomer rubber and 12.5 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro powder mill for grinding for 2.5h, then sieving with a 1250-mesh sieve, and collecting to prepare TPU coated nano copper powder filler; the three-ring micronizer is ZYM80 three-ring micronizer in ZYM, with spindle rotation speed of 240r/min, grinding rings number of 3, and grinding rollers number of 20;
(3) adding polyether polyol into a closed reaction kettle, heating to 80 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding pigment filler, plasticizer and other auxiliaries, continuously heating to 115 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the polyether polyol is polytetrahydrofuran polyether polyol; the pigment and filler is talcum powder; the plasticizer is dioctyl phthalate; the other auxiliary agents are a mixture prepared from a defoaming agent BYK-064, a dispersing agent DY-9006 and an antioxidant T-501 according to a mass ratio of 1:0.8: 1.4; the vacuum degree of vacuum dehydration is-0.095 MPa, and the time is 2.5 h;
the raw materials comprise, by weight, 30 parts of polyether polyol, 5 parts of TPU coated nano copper powder filler, 5 parts of pigment filler, 8 parts of plasticizer and 0.6 part of other auxiliary agents;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 35 ℃, adding isocyanate, stirring and reacting for 1.5h, heating to 80 ℃, and continuously stirring and reacting for 4h to obtain a mixture A; the isocyanate is isophorone diisocyanate, and the adding amount of the isocyanate is 1 time of the weight of the polyether polyol;
(5) cooling the mixture A obtained in the step (4) to 40 ℃, adding a solvent and a latent curing agent, continuously stirring for 1.5h, cooling to 35 ℃, introducing inert gas for protection for 75min, and discharging to obtain a single-component polyurethane waterproof coating; the solvent is No. 150 solvent oil; the latent curing agent is 2, 2-dihydrooxazolidine; the inert gas is argon;
the raw material mixture ratio is, by weight, mixture A55 parts, solvent 12 parts, latent curing agent 0.6 parts.
The polyurethane root-blocking waterproof coating prepared in example 6 has the root-blocking performance shown in table 1.
Comparative example 1
Comparative example 1 the polyurethane elastomer is not used for coating the nano copper, the nano copper is directly added into the formula of the polyurethane waterproof coating, other preparation conditions and proportions are the same as those of example 6, and the prepared polyurethane root-resistant waterproof coating has the root-resistant performance shown in table 1.
The performance index testing method comprises the following steps:
root resistance: the polyurethane waterproof coatings prepared in the embodiments 1-6 and the comparative example 1 are coated on the bottom of a ceramic groove with an opening at the upper part of 60 multiplied by 60cm, 10 ceramic grooves are coated in each group, soil with the same texture and the height of 40cm is added into each groove, a pyracantha fortuneana with similar growth vigor is planted in each groove, the distance between the root of the pyracantha fortuneana and the waterproof coating is kept at 5cm, cultivation is carried out in the same environment according to the growth habit of the pyracantha fortuneana, and the conditions of the root system, branches and leaves and the waterproof coating are observed after normal cultivation for 6 months.
As can be seen from table 1: according to the comparative example, after the nano copper powder which is not coated by the TPU is added into the polyurethane waterproof coating, the waterproof layer cracks due to the phase separation with the polyurethane waterproof coating, and meanwhile, due to the problem of poor dispersibility of the nano copper powder in the coating, part of coating areas have no root blocking copper powder, so that a plant root system penetrates into the waterproof coating layer, and the water leakage condition of the waterproof coating layer is caused. Since the comparative examples and the examples have no influence on plants, the nano copper powder has the effect of root resistance and has no influence on the plants. The root penetration resistant waterproof coating prepared by the invention has good root resistance, low price and simple production process, and is suitable for large-scale production.
Table 1:
| property of (2) Can be used for Finger-shaped Sign board | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example 1 |
| Root of herbaceous plant Wearing device Thorn Love of a person In a state of being immersed in | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Do not grow into Water layer, prevention of The water layer is intact | 10 lines of roots Growing in a small amount Waterproof, waterproof Crack in water layer Line(s) |
| Plant (CN) Article (A) Root of herbaceous plant Is a system Love of a person In a state of being immersed in | Without withering | Without withering | Without withering | Without withering | Without withering | Without withering | Without withering |
| Plant (CN) Article (A) Leaf of Chinese character Seed of Japanese apricot Love of a person In a state of being immersed in | Without withering | Without withering | Without withering | Without withering | Without withering | Without withering | Without withering |
Claims (10)
1. A preparation method of a polyurethane root-resistant waterproof coating is characterized by comprising the following specific steps:
(1) firstly, adding thermoplastic polyurethane elastomer rubber (TPU) into a screw extruder, setting the temperature of each heating section of a screw and the rotation speed parameter of the screw, then heating under the protection of nitrogen to melt the TPU elastomer rubber, then slowly adding nano copper powder into a second feeding port, uniformly mixing, extruding, granulating and discharging to obtain TPU coated nano copper powder; the raw materials comprise, by weight, 100-120 parts of thermoplastic polyurethane elastomer rubber and 10-15 parts of nano copper powder;
(2) adding the TPU coated nano copper powder prepared in the step (1) into a three-ring micro powder mill for grinding for 2-3 h, then sieving with a 1250-mesh sieve, and collecting to prepare the TPU coated nano copper powder filler;
(3) adding polyether polyol into a closed reaction kettle, heating to 70-90 ℃, then adding the TPU coated nano copper powder filler prepared in the step (2), mixing and stirring uniformly, adding the pigment filler, the plasticizer and other auxiliaries, continuously heating to 100-130 ℃, and carrying out vacuum dehydration to obtain a uniformly mixed raw material; the raw materials comprise, by weight, 20-40 parts of polyether polyol, 5-10 parts of TPU coated nano copper powder filler, 3-5 parts of pigment filler, 5-10 parts of plasticizer and 0.3-0.8 part of other additives;
(4) cooling the uniformly mixed raw material obtained in the step (3) to 30-40 ℃, adding isocyanate, stirring and reacting for 1-2 hours, heating to 60-100 ℃, and continuously stirring and reacting for 3-5 hours to obtain a mixture A;
(5) cooling the mixture A obtained in the step (4) to 30-50 ℃, adding a solvent and a latent curing agent, continuously stirring for 1-2 hours, cooling to 30-40 ℃, introducing an inert gas for protection for 50-100 min, and discharging to obtain a single-component polyurethane waterproof coating; the raw material mixture ratio is, by weight, 10-15 parts of a solvent, 0.4-1 part of a latent curing agent and 30-80 parts of a mixture A.
2. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the thermoplastic polyurethane elastomer rubber in the step (1) is TPU 9852D.
3. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the screw extruder in the step (1) is one of a single screw extruder, a double screw extruder and a three-screw extruder, the length-diameter ratio of screws is 20-30, and the rotating speed is 100-120 r/min; the temperature of each heating section of the screw extruder is 150-160 ℃ in the feeding section, 180-210 ℃ in the melting section and 170-180 ℃ in the homogenizing section.
4. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the particle size of the nano copper powder in the step (1) is 20-100 nm, and the feeding speed of the nano copper powder in a screw extruder is 50-200 g/min.
5. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: and (3) the three-ring micro-powder mill in the step (2) is ZYM three-ring micro-powder mill in Zodiac, the specific model can be ZYM80, the rotating speed of a main shaft is 235-240 r/min, the number of grinding rings is 3, and the number of grinding rollers is 20.
6. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the polyether polyol in the step (3) is at least one of PPG polyether polyol, POP polymer polyether polyol and polytetrahydrofuran polyether polyol, and the molecular weight is 500-5000; the pigment and filler is at least one of carbon black, titanium dioxide, iron yellow, kaolin, wollastonite and talcum powder; the plasticizer is one of dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, chlorinated paraffin and citric acid ester; the other auxiliary agents are a mixture prepared from a defoaming agent, a dispersing agent and an antioxidant according to the mass ratio of 1: 0.5-1: 0.8-2, wherein the defoaming agent is BYK-064, the dispersing agent is DY-9006, and the antioxidant is T-501.
7. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: and (3) the vacuum degree of the vacuum dehydration is-0.09 to-0.1 MPa, and the time is 2 to 3 hours.
8. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the isocyanate in the step (4) is one of 1, 6-hexamethylene diisocyanate and isophorone diisocyanate, and the adding amount of the isocyanate is 0.8-1.2 times of the weight of the polyether polyol.
9. The preparation method of the polyurethane root-resistant waterproof coating material according to claim 1, characterized in that: the solvent in the step (5) is 150# solvent oil; the latent curing agent is one of 2-isopropyl-N-hydroxyethyl-oxazolidine, 2-isopropyl oxazolidine and 2, 2-dihydro oxazolidine; the inert gas is one of helium, neon and argon.
10. A polyurethane root-resistant waterproof coating prepared by the method of any one of claims 1 to 9.
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| CN112646431A (en) * | 2021-01-08 | 2021-04-13 | 常州回天新材料有限公司 | Printing coating for photovoltaic module and preparation method thereof |
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