CN111909611A - High-elongation anti-sagging polyurethane waterproof coating and preparation method thereof - Google Patents
High-elongation anti-sagging polyurethane waterproof coating and preparation method thereof Download PDFInfo
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- CN111909611A CN111909611A CN202010835772.2A CN202010835772A CN111909611A CN 111909611 A CN111909611 A CN 111909611A CN 202010835772 A CN202010835772 A CN 202010835772A CN 111909611 A CN111909611 A CN 111909611A
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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Abstract
The invention relates to the field of waterproof coatings, and discloses a high-elongation anti-sagging polyurethane waterproof coating and a preparation method thereof. The preparation method comprises the following preparation processes: (1) adding sodium bentonite and diallyl dimethyl ammonium chloride into water, heating, stirring and reacting to obtain diallyl dimethyl ammonium chloride modified bentonite; (2) adding diallyl dimethyl ammonium chloride modified bentonite, hydroxyethyl acrylate and an initiator into water, heating and stirring for reaction to prepare an organic modified bentonite anti-sagging agent; (3) mixing polyether polyol, pigment and filler and isocyanate, controlling the temperature, stirring for reaction, and then uniformly mixing with a chain extender, a defoaming agent, a latent curing agent, a catalyst and an organic modified bentonite anti-sagging agent to obtain the high-elongation anti-sagging polyurethane waterproof coating. According to the invention, by introducing the polyhydroxyethyl acrylate on the surface of the sodium bentonite, the prepared coating has good sagging resistance, high elongation and wide application prospect.
Description
Technical Field
The invention relates to the field of waterproof coatings, and discloses a high-elongation anti-sagging polyurethane waterproof coating and a preparation method thereof.
Background
The polyurethane waterproof paint is one kind of single component waterproof polyurethane paint prepared with isocyanate group-containing prepolymer prepared through addition polymerization of isocyanate, polyether, etc. and through mixing with catalyst, anhydrous assistant, anhydrous stuffing, solvent, etc. The paint is a reaction curing type (moisture curing) paint and has the characteristics of high strength, high elongation, good water resistance and the like. The adaptability to the deformation of the base layer is strong. At present, polyurethane waterproof paint becomes popular water-based environment-friendly waterproof paint.
The polyurethane waterproof coating is a single-component environment-friendly waterproof coating for liquid construction, a polyurethane coating film contains a large amount of urea bonds and urethane bonds, and due to the action of hydrogen bonds and the like, the coating film has excellent adhesive force, wear resistance, oil resistance, acid and alkali resistance, impact resistance and good electrical insulation. However, the prior art also has the following problems: the drying speed is too slow. The final hardness can not be achieved within a plurality of days at normal temperature, the products are easy to adhere when being stacked, the requirements of industrial high-quality and high-efficiency coating can not be met, and the construction problems of whitening, cracking, uneven gloss, easy sagging and the like are particularly easy to occur. The coating has the advantages that the coating is easy to sag, and the construction efficiency and the construction quality of the coating are seriously affected.
Currently, the anti-sagging single-component polyurethane waterproof coating suitable for facade construction, which is put on the market, generally adopts fumed silica, organic bentonite, polyamide wax powder and the like as anti-sagging agents (thixotropic agents), and the traditional thixotropic agents have large addition amount, can be uniformly dispersed only by high shearing force during production, and have high requirements on production equipment. In recent years, studies on sag resistant polyurethane waterproof coatings have been increasing.
The Chinese patent application No. 201611225116.0 discloses an anti-sagging single-component polyurethane waterproof paint and a preparation method thereof, wherein an anti-sagging agent of the polyurethane waterproof paint is hyperbranched polyurea formed by reacting hyperbranched polyethyleneimine with a monoisocyanate-terminated prepolymer, wherein the molecular structure of the hyperbranched polyethyleneimine contains 10-30 nitrogen atoms, and the monoisocyanate-terminated prepolymer is obtained by reacting a diisocyanate monomer with 3-12 monohydric alcohol.
The Chinese patent application No. 201811061165.4 discloses a preparation method of a single-component anti-sagging polyurethane waterproof coating, which comprises the following steps: (1) mixing the dehydrated polyether polyol with first isocyanate under the protection of inert gas, and reacting to obtain a polyurethane prepolymer; (2) premixing the polyurethane prepolymer with the dehydrated modified nano calcium carbonate, polyurea, modified nano fumed silica and filler, adding the mixture into a first twin-screw extruder, mixing and dispersing, and extruding to obtain a dispersed mixture, wherein the polyurea is prepared by reacting second isocyanate and diamine; (3) and adding the dispersed mixture into a second double-screw extruder, sequentially adding a solvent and an auxiliary agent, mixing, dispersing and extruding to obtain the single-component anti-sagging polyurethane waterproof coating.
According to the above, the polyurethane waterproof coating in the existing scheme has the problem of easy sagging, and the method for enhancing the sagging resistance of the polyurethane coating by using the sagging resistant agent such as organic bentonite and the like has the advantages that the added bentonite reduces the elongation of the coating, so that brush lines can be left in the coating process, the coating surface is not attractive, and the application of the coating is influenced.
Disclosure of Invention
At present, the method for improving the anti-sagging performance of the polyurethane waterproof coating by using the anti-sagging agents such as organic bentonite and the like is widely applied, and the problem of the reduction of the elongation of the coating caused by the addition of the organic bentonite is solved.
The invention solves the problems through the following technical scheme:
a preparation method of a high-elongation anti-sagging polyurethane waterproof coating comprises the following specific steps:
(1) adding sodium bentonite into water, ultrasonically dispersing uniformly, adding diallyl dimethyl ammonium chloride, stirring, heating to 75-85 ℃, stirring at a constant temperature at a rotating speed of 200-300 r/min for reacting for 3-4 h, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 60-80 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 200-300 r/min for 3-4 h, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 100-130 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 40-60 ℃, adding an isocyanate monomer under the protection of nitrogen, stirring and reacting at 75-85 ℃ for polymerization for 2-3 h, cooling to 30-50 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing at the rotating speed of 300-500 r/min for 20-40 min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating.
According to the invention, sodium bentonite is selected as the anti-sagging agent, and the sodium bentonite is added into the polyurethane coating, so that a gel structure can be formed in the coating through a hydrogen bond, and the anti-sagging performance of the coating is effectively improved. As a preferable mode of the invention, the sodium bentonite in the step (1) is sodium bentonite produced by Xinyu bentonite.
The diallyl dimethyl ammonium chloride is used as a modified material, and the molecular structure of the diallyl dimethyl ammonium chloride contains alkenyl double bonds, so that linear homopolymers and various copolymers can be formed through various polymerization reactions, and meanwhile, the diallyl dimethyl ammonium chloride with high electropositivity can generate high electrostatic interaction with bentonite and be adsorbed on the surface of the bentonite, and double bonds are introduced on the surface of sodium bentonite, so that the surface of the organically modified bentonite has double bond active groups, and the organic material with high elongation is conveniently introduced on the surface through subsequent polymerization reactions. Preferably, the raw materials in the step (1) comprise, by weight, 10-15 parts of sodium bentonite, 100-150 parts of water and 3-8 parts of diallyl dimethyl ammonium chloride.
Adding diallyl dimethyl ammonium chloride modified bentonite, hydroxyethyl acrylate and an initiator into water for polymerization reaction. The invention initiates polymerization reaction on the surface of the organically modified bentonite with double-bond active groups on the surface, grafts the long-chain polyhydroxyethyl acrylate on the surface of the modified bentonite through free radical polymerization reaction, increases the organic chain segment on the surface of the bentonite, improves the elongation of the bentonite, and further ensures the anti-sagging property of the coating and the elongation of the coating. In addition, the polyhydroxyethyl acrylate and the polyamino acid prepolymer have good compatibility, so that the modified bentonite can be well dispersed in the polyurethane, and the modification effect is effectively ensured.
The initiator is selected from a redox initiation system initiator, and two initiators with oxidizability and reducibility generate free radicals through redox reaction, so that the monomer polymerization is initiated. Preferably, the initiator in step (2) is a redox system initiator; in a further preferred embodiment of the present invention, the redox initiator may be one of ammonium persulfate and sodium bisulfite.
Preferably, the raw materials in the step (2) comprise, by weight, 10-20 parts of diallyl dimethyl ammonium chloride modified bentonite, 100-150 parts of water, 6-10 parts of hydroxyethyl acrylate and 0.05-0.1 part of an initiator.
Preferably, the polyether polyol in step (3) is at least one of polyether diol and polyether triol.
In a preferred embodiment of the present invention, the isocyanate in step (3) is at least one of toluene diisocyanate and diphenylmethane diisocyanate.
Preferably, the pigment and filler in step (3) is one of titanium dioxide, heavy calcium carbonate and kaolin.
Preferably, the chain extender in the step (3) is diethyltoluenediamine.
Preferably, the defoaming agent in the step (3) is at least one of polysiloxane defoaming agent, silicone defoaming agent, calcium hydroxide and magnesium oxide.
In the present invention, the latent curing agent in the step (3) is preferably an oxazolidine curing agent.
Preferably, in the step (3), the catalyst is one of dibutyltin dilaurate, stannous octoate and triethylenediamine.
Preferably, the vacuum pressure of the vacuum dehydration in the step (3) is-0.09 to-0.1 MPa, and the time is 1 to 2 hours.
Preferably, in the step (3), the raw materials comprise, by weight, 40-50 parts of polyether polyol, 10-20 parts of pigment and filler, 20-30 parts of isocyanate, 0.3-0.6 part of chain extender, 0.4-1 part of defoamer, 1-5 parts of latent curing agent, 0.2-0.5 part of catalyst and 0.6-3 parts of organic modified bentonite anti-sagging agent.
The anti-sagging polyurethane waterproof coating with high elongation rate prepared by the method has good anti-sagging performance and high elongation rate, so that the coating does not have lines after being coated, and the surface of the coating after being coated is more attractive.
The invention provides a high-elongation anti-sagging polyurethane waterproof coating and a preparation method thereof, which comprises the steps of adding sodium bentonite into water, performing ultrasonic dispersion, continuously adding diallyl dimethyl ammonium chloride, stirring and heating, stirring and reacting at constant temperature, cooling, and performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; adding the obtained diallyl dimethyl ammonium chloride modified bentonite into water for dispersion, continuously adding hydroxyethyl acrylate, stirring and heating, adding an initiator, stirring and reacting at a constant temperature, performing centrifugal separation, drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating, starting a vacuum pump for dehydration, then cooling, introducing nitrogen for protection, adding an isocyanate monomer, stirring and controlling the temperature for polymerization, adding a chain extender, a defoaming agent, a latent curing agent and a catalyst after cooling, stirring and mixing uniformly, adding the obtained organic modified bentonite anti-sagging agent into the reaction kettle, and stirring and dispersing uniformly.
The invention provides a high-elongation anti-sagging polyurethane waterproof coating and a preparation method thereof, and compared with the prior art, the high-elongation anti-sagging polyurethane waterproof coating has the outstanding characteristics and excellent effects that:
1. provides a method for preparing anti-sagging polyurethane waterproof coating with high elongation by introducing polyhydroxyethyl acrylate on the surface of sodium bentonite.
2. Double bonds are introduced to the surface of the conventional anti-sagging bentonite, the organic chain segment on the surface of the bentonite is increased through free radical polymerization, and the long-chain polyhydroxyethyl acrylate is grafted to the surface of the modified bentonite, so that the elongation of the bentonite is improved, the elongation of the coating can be ensured while the anti-sagging performance of the coating is improved, and brush marks on the surface of the coating due to low elongation of the coating after coating are prevented.
3. According to the invention, the polyhydroxyethyl acrylate introduced on the surface of the bentonite has better compatibility with the polyamino acid prepolymer, so that the modified bentonite can be better dispersed in polyurethane, the anti-sagging performance and the high-elongation effect of the coating are ensured, the coating does not have lines after being coated, and the surface of the coating after being coated is more attractive.
Drawings
Fig. 1 shows the sagging condition of the polyurethane waterproof coating prepared in comparative example 1 after being coated and dried according to the test method, wherein ↓ represents the sagging length.
Fig. 2 shows the sagging condition of the polyurethane waterproof coating prepared in comparative example 2 after being coated and dried according to the test method, wherein ↓ represents the sagging length.
Fig. 3 shows the sagging condition of the polyurethane waterproof coating prepared in example 6 after being coated and dried according to the test method, wherein ↓ represents the sagging length.
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 sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 78 ℃, stirring and reacting for 3.5 hours at constant temperature at the rotating speed of 260r/min, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise, by weight, 13 parts of sodium bentonite, 130 parts of water and 5 parts of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 68 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 260r/min for 3.5 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is ammonium persulfate;
the raw materials comprise, by weight, 16 parts of diallyl dimethyl ammonium chloride modified bentonite, 130 parts of water, 9 parts of hydroxyethyl acrylate and 0.07 part of an initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 120 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 48 ℃, adding an isocyanate monomer under the protection of nitrogen, controlling the temperature to 78 ℃, stirring, reacting and polymerizing for 2.5 hours, cooling to 38 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 28min at the rotating speed of 400r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether diol; the isocyanate is toluene diisocyanate; the pigment and filler is titanium dioxide; the chain extender is diethyl toluene diamine; the defoaming agent is a polysiloxane defoaming agent; the latent curing agent is oxazolidine curing agent; the catalyst is dibutyltin dilaurate; the vacuum pressure of the vacuum dehydration is-0.096 MPa, and the time is 1.5 h;
the raw materials comprise, by weight, 46 parts of polyether polyol, 14 parts of pigment and filler, 26 parts of isocyanate, 0.5 part of chain extender, 0.8 part of defoaming agent, 4 parts of latent curing agent, 0.3 part of catalyst and 2.1 parts of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproof coating obtained in example 1 are shown in table 1.
Example 2
(1) Firstly, adding sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 76 ℃, stirring and reacting for 4 hours at constant temperature at a rotating speed of 220r/min, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise, by weight, 11 parts of sodium bentonite, 140 parts of water and 4 parts of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 65 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 220r/min for 4 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is ammonium persulfate;
the raw materials comprise, by weight, 13 parts of diallyl dimethyl ammonium chloride modified bentonite, 140 parts of water, 7 parts of hydroxyethyl acrylate and 0.06 part of an initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 110 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 45 ℃, adding an isocyanate monomer under the protection of nitrogen, stirring and reacting at 78 ℃ for polymerization for 3 hours, cooling to 35 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 35 minutes at the rotating speed of 350r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether triol; the isocyanate is diphenylmethane diisocyanate; the pigment and filler is heavy calcium carbonate; the chain extender is diethyl toluene diamine; the defoaming agent is a silicone defoaming agent; the latent curing agent is oxazolidine curing agent; the catalyst is stannous octoate; the vacuum pressure of the vacuum dehydration is-0.09 MPa, and the time is 2 h;
the raw materials comprise, by weight, 48 parts of polyether polyol, 12 parts of pigment and filler, 28 parts of isocyanate, 0.4 part of chain extender, 0.5 part of defoamer, 2 parts of latent curing agent, 0.3 part of catalyst and 1 part of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproof coating obtained in example 2 are shown in table 1.
Example 3
(1) Firstly, adding sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 82 ℃, stirring and reacting at constant temperature at a rotating speed of 280r/min for 3 hours, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise, by weight, 14 parts of sodium bentonite, 110 parts of water and 7 parts of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 75 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 280r/min for 3 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is sodium bisulfite;
the raw materials comprise, by weight, 18 parts of diallyl dimethyl ammonium chloride modified bentonite, 110 parts of water, 9 parts of hydroxyethyl acrylate and 0.09 part of an initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 125 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 55 ℃, adding an isocyanate monomer under the protection of nitrogen, stirring and reacting at 82 ℃ for polymerization for 2 hours, cooling to 45 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 25 minutes at the rotating speed of 450r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether diol; the isocyanate is toluene diisocyanate; the pigment and filler is kaolin; the chain extender is diethyl toluene diamine; the defoaming agent is calcium hydroxide; the latent curing agent is oxazolidine curing agent; the catalyst is triethylene diamine; the vacuum pressure of the vacuum dehydration is-0.1 MPa, and the time is 1 h;
the raw materials comprise, by weight, 42 parts of polyether polyol, 18 parts of pigment and filler, 23 parts of isocyanate, 0.5 part of chain extender, 0.8 part of defoamer, 4 parts of latent curing agent, 0.4 part of catalyst and 2 parts of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproof coating obtained in example 3 are shown in table 1.
Example 4
(1) Firstly, adding sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 75 ℃, stirring and reacting for 4 hours at a constant temperature at a rotating speed of 200r/min, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise, by weight, 10 parts of sodium bentonite, 150 parts of water and 3 parts of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 60 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 200r/min for 4 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is sodium bisulfite;
the raw materials comprise, by weight, 10 parts of diallyl dimethyl ammonium chloride modified bentonite, 150 parts of water, 6 parts of hydroxyethyl acrylate and 0.05 part of an initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 100 ℃, then starting a vacuum pump to perform vacuum dehydration, cooling to 40 ℃, adding an isocyanate monomer under the protection of nitrogen, stirring and reacting at 75 ℃ for polymerization for 3 hours, cooling to 30 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 40min at the rotating speed of 300r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether triol; the isocyanate is diphenylmethane diisocyanate; the pigment and filler is titanium dioxide; the chain extender is diethyl toluene diamine; the defoaming agent is magnesium oxide; the latent curing agent is oxazolidine curing agent; the catalyst is dibutyltin dilaurate; the vacuum pressure of the vacuum dehydration is-0.09 MPa, and the time is 2 h;
the raw materials comprise, by weight, 50 parts of polyether polyol, 10 parts of pigment and filler, 30 parts of isocyanate, 0.3 part of chain extender, 0.4 part of defoamer, 1 part of latent curing agent, 0.2 part of catalyst and 0.6 part of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproofing paint prepared in example 4 are shown in table 1.
Example 5
(1) Firstly, adding sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 85 ℃, then stirring and reacting at a constant temperature at a rotating speed of 300r/min for 3 hours, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise 15 parts by weight of sodium bentonite, 100 parts by weight of water and 8 parts by weight of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 80 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 300r/min for 3 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is ammonium persulfate;
the raw materials comprise, by weight, 20 parts of diallyl dimethyl ammonium chloride modified bentonite, 100 parts of water, 10 parts of hydroxyethyl acrylate and 0.1 part of initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 130 ℃, then starting a vacuum pump to perform vacuum dehydration, cooling to 60 ℃, then adding an isocyanate monomer under the protection of nitrogen, controlling the temperature to 85 ℃, stirring and reacting for polymerization for 2 hours, cooling to 50 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 20 minutes at the rotating speed of 500r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether diol; the isocyanate is diphenylmethane diisocyanate; the pigment and filler is heavy calcium carbonate; the chain extender is diethyl toluene diamine; the defoaming agent is a polysiloxane defoaming agent; the latent curing agent is oxazolidine curing agent; the catalyst is stannous octoate; the vacuum pressure of the vacuum dehydration is-0.1 MPa, and the time is 1 h;
the raw materials comprise, by weight, 40 parts of polyether polyol, 20 parts of pigment and filler, 20 parts of isocyanate, 0.6 part of chain extender, 1 part of defoamer, 5 parts of latent curing agent, 0.5 part of catalyst and 3 parts of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproof coating obtained in example 5 are shown in table 1.
Example 6
(1) Firstly, adding sodium bentonite into water, performing ultrasonic dispersion uniformly, then adding diallyl dimethyl ammonium chloride, stirring and heating to 80 ℃, then stirring and reacting at a constant temperature at a rotating speed of 250r/min for 3.5h, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite; the sodium bentonite is produced from Xinyu bentonite;
the raw materials comprise, by weight, 12.5 parts of sodium bentonite, 125 parts of water and 5.5 parts of diallyl dimethyl ammonium chloride;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 70 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 250r/min for 3.5 hours, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent; the initiator is sodium bisulfite;
the raw materials comprise, by weight, 15 parts of diallyl dimethyl ammonium chloride modified bentonite, 125 parts of water, 8 parts of hydroxyethyl acrylate and 0.08 part of an initiator;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 115 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 50 ℃, then adding an isocyanate monomer under the protection of nitrogen, controlling the temperature to be 80 ℃, stirring, reacting and polymerizing for 2.5 hours, cooling to 40 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing for 30min at the rotating speed of 400r/min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating; the polyether polyol is polyether triol; the isocyanate is toluene diisocyanate; the pigment and filler is kaolin; the chain extender is diethyl toluene diamine; the defoaming agent is a silicone defoaming agent; the latent curing agent is oxazolidine curing agent; the catalyst is triethylene diamine; the vacuum pressure of the vacuum dehydration is-0.095 MPa, and the time is 1.5 h;
the raw materials comprise, by weight, 45 parts of polyether polyol, 15 parts of pigment and filler, 25 parts of isocyanate, 0.45 part of chain extender, 0.6 part of defoamer, 3 parts of latent curing agent, 0.4 part of catalyst and 1.8 parts of organic modified bentonite anti-sagging agent.
The thickness, the dried state, the viscosity, the sagging degree and the precipitation of the polyurethane waterproof coating obtained in example 6 are shown in table 1.
Comparative example 1
Comparative example 1 no hydroxyethyl acrylate-modified bentonite was used, and the preparation conditions were the same as in example 6, and the thickness, the state after air-drying, the viscosity, the sag and the precipitation of the obtained polyurethane waterproofing paint were as shown in table 1.
Comparative example 2
Comparative example 2 no organic modified bentonite anti-sagging agent was added and the preparation conditions were the same as in example 6, and the thickness, the state after air-drying, the viscosity, the sag and the precipitation of the prepared polyurethane waterproof coating material were as shown in table 1.
The performance index testing method comprises the following steps:
the polyurethane waterproof coating prepared in the embodiments 1-6 and the comparative examples 1-2 is applied to a wall surface which is 1m away from the ground and is cleaned, the coating area of each sample is 100 multiplied by 100cm, the coating is waited to be dried after one-time coating, the thickness of the coating is measured, the sag after coating is tested, the viscosity of the coating is measured, and whether precipitation is generated or not is observed.
As can be seen from table 1 and fig. 1, 2 and 3, whether the addition of the anti-sagging agent has little effect on the viscosity of the coating, as can be seen from comparative example 1 and example 6, the bentonite which is not modified with hydroxyethyl acrylate also has the anti-sagging effect as shown in fig. 1, but the surface of the coating after drying shows a small amount of brush mark lines due to the low elongation of the coating, while comparative example 2 does not add the bentonite anti-sagging agent, which has large sagging after coating and is remarkable in sagging, as shown in fig. 2. Therefore, the method of the invention not only has good anti-sagging performance by modifying the bentonite with acrylic acid, but also ensures that the coating does not have lines after being coated and the surface of the coating is more beautiful after being coated by improving the elongation of the bentonite.
Table 1:
Claims (10)
1. a preparation method of a high-elongation anti-sagging polyurethane waterproof coating is characterized by comprising the following specific steps:
(1) adding sodium bentonite into water, ultrasonically dispersing uniformly, adding diallyl dimethyl ammonium chloride, stirring, heating to 75-85 ℃, stirring at a constant temperature at a rotating speed of 200-300 r/min for reacting for 3-4 h, cooling after the reaction is finished, and finally performing centrifugal separation to obtain diallyl dimethyl ammonium chloride modified bentonite;
(2) firstly, adding the diallyl dimethyl ammonium chloride modified bentonite obtained in the step (1) into water, performing ultrasonic dispersion uniformly, then adding hydroxyethyl acrylate, stirring and heating to 60-80 ℃, adding an initiator, stirring and reacting at a constant temperature at a rotating speed of 200-300 r/min for 3-4 h, performing centrifugal separation after the reaction is finished, and drying and dehydrating to obtain the organic modified bentonite anti-sagging agent;
(3) adding polyether polyol and pigment filler into a closed reaction kettle, stirring and heating to 100-130 ℃, then starting a vacuum pump for vacuum dehydration, cooling to 40-60 ℃, adding an isocyanate monomer under the protection of nitrogen, stirring and reacting at 75-85 ℃ for polymerization for 2-3 h, cooling to 30-50 ℃ after the reaction is finished, simultaneously adding a chain extender, a defoaming agent, a latent curing agent and a catalyst, stirring and mixing uniformly, finally adding the organic modified bentonite anti-sagging agent prepared in the step (2) into the reaction kettle, stirring and dispersing at the rotating speed of 300-500 r/min for 20-40 min, and thus obtaining the high-elongation anti-sagging polyurethane waterproof coating.
2. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the sodium bentonite in the step (1) is produced from Xinyu bentonite.
3. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the raw materials in the step (1) comprise, by weight, 10-15 parts of sodium bentonite, 100-150 parts of water and 3-8 parts of diallyl dimethyl ammonium chloride.
4. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the initiator in the step (2) is a redox system initiator, and specifically can be one of ammonium persulfate and sodium bisulfite.
5. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the raw materials in the step (2) comprise, by weight, 10-20 parts of diallyl dimethyl ammonium chloride modified bentonite, 100-150 parts of water, 6-10 parts of hydroxyethyl acrylate and 0.05-0.1 part of an initiator.
6. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the polyether polyol in the step (3) is at least one of polyether diol and polyether triol; the isocyanate is at least one of toluene diisocyanate and diphenylmethane diisocyanate.
7. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the pigment filler in the step (3) is one of titanium dioxide, heavy calcium carbonate and kaolin; the chain extender is diethyl toluene diamine; the defoaming agent is at least one of polysiloxane defoaming agent, silicone defoaming agent, calcium hydroxide and magnesium oxide; the latent curing agent is oxazolidine curing agent; the catalyst is one of dibutyltin dilaurate, stannous octoate and triethylenediamine.
8. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: and (3) performing vacuum dehydration under the vacuum pressure of-0.09 to-0.1 MPa for 1 to 2 hours.
9. The preparation method of the high-elongation anti-sagging polyurethane waterproof coating according to claim 1, characterized in that: the raw materials in the step (3) comprise, by weight, 40-50 parts of polyether polyol, 10-20 parts of pigment and filler, 20-30 parts of isocyanate, 0.3-0.6 part of chain extender, 0.4-1 part of defoamer, 1-5 parts of latent curing agent, 0.2-0.5 part of catalyst and 0.6-3 parts of organic modified bentonite anti-sagging agent.
10. A high-elongation anti-sagging polyurethane waterproof coating prepared by the method of any one of claims 1 to 9.
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| CN114574089A (en) * | 2022-03-01 | 2022-06-03 | 江苏雨中情防水材料有限责任公司 | Single-component polyurethane waterproof coating capable of being formed by one-step construction and application thereof |
| CN114605887A (en) * | 2022-04-19 | 2022-06-10 | 宁波宣威彩色世界涂料有限公司 | Smooth, clean and odor-free super-scrubbing water paint for skin |
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