Solvent-free polyurethane floating color sand self-leveling floor material and preparation method thereof

Abstract

The application discloses a kind of solventless polyurethane floating color sand self-leveling floor materials and preparation method, including component A, component B, component C, component D;The mass ratio of each component is as follows: component A: component B: component C: component D=1~1.5:0.5~1:0.3~0.6:0.3~0.6;Component A is polyol resin mixture, auxiliary agent and pigment and filler etc.;Component B is isocyanate blend;Component C is resin color sand;Component D is quartz sand.The self-leveling floor material of the application realizes the thick coating type solventless polyurethane self-leveling of one-time coating forming, and the maximum construction thickness can reach 3mm, with high efficiency, fast curing, 24h after construction at 25 DEG C can be walked;After curing, resin color sand floats on the surface layer of material, with strong color sand texture, very decorative and wear resistance, is the ideal industrial floor material of new energy automobile, electronics and chemical workshop, food plant, pharmaceutical factory, airport, hospital etc..

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of polyurethane floor materials, in particular to a solvent-free polyurethane floating color sand self-leveling floor material and a preparation method thereof. BACKGROUND

[0002] With the continuous iteration and update of technology, the requirements of modern industry on floor materials are also becoming more and more demanding, especially in the new energy automobile, electronics, medical, food and chemical industries; the floor is required to be dustproof and anti-skid, high pressure-resistant and high mechanical wear-resistant, free of volatile harmful substances, excellent in corrosion resistance, flat and comfortable, resistant to dirt, and also has certain decorative performance. At the same time, under the double pressure of work rhythm and industry competition, modern industry also has higher requirements on the efficiency of floor construction, so that the floor is simple to construct, rapid to form, and high in application efficiency, which has gradually become a popular choice. Therefore, it is the common expectation to launch a high-end floor material that can combine the above requirements of modern industry on floor materials, can be quickly formed and applied.

[0003] Color sand floor material is a kind of floor material that resin is freely matched with different color sands to present bright and colorful colors, which is extremely decorative. Although epoxy resin sand pressing floor has good decorative effect and can resist heavy load, the construction process is complex, the steps are cumbersome, and the construction efficiency is low, and in the application environment of high temperature, high humidity, organic acid and alkali corrosion, the performance is obviously affected. The epoxy floating color sand self-leveling material adds resin floating color sand with brighter color, has better decorative effect and one-time construction forming, although it solves the problem of low construction efficiency of epoxy sand pressing color sand floor, but since the base resin is still epoxy resin, the floor material is still difficult to be applied in the above harsh environment for a long time.

[0004] CN115010403 discloses a water-based polyurethane floating colored sand self-leveling mortar and its preparation process. Compared with ordinary water-based polyurethane mortar self-leveling material, although melamine resin floating colored sand is added for decoration, it has the properties of polyurethane such as high temperature resistance, high humidity resistance, and resistance to organic acid, alkali and the like. However, due to the composite of water-based polyurethane and cement mortar, the system has poor resistance to heavy load and compression, and poor dirt resistance. Moreover, the addition amount of the floating colored sand is very low, and the floor material cannot exhibit the texture of the colored sand floor, and the decorative performance of the colored sand is sharply decreased. In the article "Polyurethane Colored Sand Floor" published by Zhou Fubai, Jiang Chen and Li Guorong in Surface Finishing, the preparation and construction of polyurethane colored sand floor are realized, and the floor has good decorative performance of colored sand, but it is a pressed sand floor, and the construction process is complex and low in efficiency. CN111187566A discloses a solvent-free self-leveling polyurethane wear-resistant material and a preparation method thereof, which has good wear resistance, dirt resistance and good chemical resistance of polyurethane. However, the operable time is short, and the material cannot be applied thickly, the scratch resistance is only 2H, and the material cannot provide good decorative effect of floating colored sand floor. Once scratched, worn or contaminated, the decorative function and service life are obviously affected. In order to ensure the decorative performance and prolong the service life, a transparent polyurethane finish layer is generally recommended to be covered on the surface, which increases the construction steps and prolongs the construction time.

[0005] In summary, it is worth paying attention to realize a solvent-free polyurethane floating colored sand self-leveling floor material which has good construction, decoration, compression resistance, wear resistance, scratch resistance, dirt resistance, and also has good chemical resistance, high and low temperature resistance. SUMMARY

[0006] The purpose of the present application is to provide a solvent-free polyurethane floating colored sand self-leveling floor material and a preparation method to solve the above problems. The floor material realizes one-time thick coating forming of the solvent-free polyurethane self-leveling material, and is matched with lighter PMMA resin colored sand as a decorative material. After the material is cured, a strong textured resin colored sand "floating sand" upper layer and a polyurethane resin and filler composite lower layer structure are formed from top to bottom, which has the advantages of high compression resistance, wear resistance, scratch resistance, corrosion resistance, dirt resistance, easy cleaning, long service life and good decoration.

[0007] The present application realizes the above-mentioned purposes through the following technical solutions:

[0008] A solvent-free polyurethane floating colored sand self-leveling floor material, comprising components A, B, C and D, and the mass ratio of each component is as follows: component A: component B: component C: component D = 1-1.5: 0.5-1: 0.3-0.6: 0.3-0.6.

[0009] The component A comprises the following materials by weight fraction: branched polyether / polyester polyol 20-30 parts by weight, refined castor oil 10-20 parts by weight, modified castor oil 5-10 parts by weight, wetting agent 0.2-0.5 parts by weight, dispersing agent 0.5-0.8 parts by weight, leveling agent 0.4-0.8 parts by weight, defoaming agent 0.3-0.6 parts by weight, water removing agent 8-12 parts by weight, filler 60-80 parts by weight, pigment 2-4 parts by weight; the component B comprises the following materials by weight fraction: branched polyether / polyester polyol modified by p-phenyl methane diisocyanate 15-25 parts by weight, polymethylene polyphenyl isocyanate 30-50 parts by weight; the component C comprises the following materials by weight fraction: resin floating color sand 25-40 parts by weight; the component D comprises the following materials by weight fraction: quartz sand 25-40 parts by weight.

[0010] Further, the branched polyether / polyester polyol in the component A is one or more of BASF Sovermol 750, Sovermol 760, Sovermol 815, Sovermol 1092, and the hydroxyl value is 200-400;

[0011] The refined castor oil is a commercially available industrial product, and the hydroxyl value is 150-175;

[0012] The modified castor oil is Ito H-31, the hydroxyl value is 157-170, and the viscosity at 25°C is less than 40 mPa.s;

[0013] The water removing agent is a commercially available high-activity nano zeolite powder; preferably, Zhengzhou Chaorong Nanometer Material CR-1274;

[0014] The filler is one or more of alumina, aluminum hydroxide, silicon powder, calcium carbonate, and mineral barium sulfate with a particle size of 600-2000;

[0015] The dispersing agent is one or more of BYK-P104S, BYK-2151, BYK-163, BYK-9076, and BYK-9011; the wetting agent is one or more of BYK-349 and BYK-3455; the leveling agent is BYK-354; and the defoaming agent is one or more of BYK-054, BYK-066N, and BYK-1794.

[0016] The pigment is a commercially available polyurethane pigment.

[0017] Further, the component B is modified by adding branched polyether / polyester polyol to modify diphenylmethane diisocyanate to obtain a modified product, wherein the branched polyether / polyester polyol is one or more of Sovermol 750, Sovermol 760, Sovermol 815, and Sovermol 1092; the diphenylmethane diisocyanate is WANNATE MDI-50; and the polymethylene polyphenyl isocyanate is one or more of WANNATE PM-200 and WANNATE PM-400.

[0018] The preparation method of the modified product is as follows: the branched polyether / polyester polyol and the diphenylmethane diisocyanate are uniformly mixed at a weight ratio of 1:4-10, and then the mixture is heated to 70-90°C in a reaction kettle with nitrogen protection and stirred for 1-1.5 h; and the modified product is obtained after cooling.

[0019] Further, the component C is dry PMMA resin colored sand particles with a particle size of 200-400 microns and a density of 1.1-1.2 g / cm 3 , and the color is red, orange, yellow, green, blue, indigo, and purple.

[0020] Further, the component D is dry 100-400 mesh quartz sand particles, preferably 140-280 mesh.

[0021] Another aspect of the present application also provides a preparation method of a solvent-free polyurethane floating colored sand self-leveling floor material, which comprises the following steps:

[0022] Step 1, preparation of the A group material: the branched polyether / polyester polyol, refined castor oil, modified castor oil, wetting agent, dispersant, water removal agent, filler, and pigment are added to a vacuum high-speed stirring dispersion machine according to the formula proportion, and then stirred and mixed at room temperature for at least 30 minutes; then the leveling agent and defoaming agent are added, and stirred and mixed at room temperature for at least 30 minutes and discharged, and then sealed and packaged to obtain the A group material; the filler should be pre-dried at 120°C for at least 1 hour for water removal treatment, and then used after cooling;

[0023] Step 2, preparation of the B group material: the branched polyether / polyester polyol and the diphenylmethane diisocyanate are uniformly mixed at a weight ratio of 1:4-10, and then heated to 70-90°C in a reaction kettle with nitrogen protection and stirred for 1-1.5 h; and the modified product is obtained after cooling; then the polymethylene polyphenyl isocyanate is added to the modified product under stirring according to the formula proportion and mixed for 0.5 h, and then sealed and packaged to obtain the B component;

[0024] Step 3, preparation of the C group material: the dry-mixed dry selected color PMMA resin colored sand is sealed and packaged to obtain the C component;

[0025] Step 4, preparation of D group material: dry quartz sand is sealed and packaged as D component;

[0026] Step 5, when in use, components A, B, C and D are mechanically mixed uniformly according to the weight ratio of component A: component B: component C: component D = 1-1.5: 0.5-1: 0.3-0.6: 0.3-0.6 to obtain a solvent-free polyurethane floating color sand self-leveling floor material.

[0027] The beneficial effects of the present application are:

[0028] The solvent-free polyurethane floating color sand self-leveling floor material of the present application realizes one-time thick coating forming of the solvent-free polyurethane self-leveling material, and has the decorative properties of colorful resin color sand; the maximum construction thickness of the floor material can reach 3 mm, and the material is fast-cured and high-efficiency, and people can walk on the floor after 24 hours of construction at 25℃; after curing, the material forms a strong-textured resin color sand "floating sand" upper layer and a polyurethane resin and filler composite lower layer structure from top to bottom, so that the floor has high compression resistance, wear resistance, scratch resistance, corrosion resistance, dirt resistance, easy cleaning and good decorative properties, and is durable.

[0029] 1) The present application uses unique high-activity nano zeolite powder as a water absorbent and adjusts its amount through a large number of tests, which not only removes the trace amount of water introduced into each component during production and storage, but also avoids the foaming problem caused by the trace amount of moisture in the air and the contact and adhesion surface of the floor material during thick coating curing; even in the hot and humid summer, the curing process is not prone to foaming, and the material is one-time formed, fast-cured and simple and efficient. The present application solves the pain point that the solvent-free polyurethane self-leveling material is difficult to be thickly coated, and makes it possible to add resin color sand to prepare a solvent-free polyurethane self-leveling color sand.

[0030] 2) The present application selects lighter PMMA resin color sand as a decorative material, which can quickly float to the surface before the gel of the solvent-free polyurethane material, forming a strong-textured "floating sand" upper layer and providing excellent decorative properties.

[0031] 3) The present application introduces low-viscosity and low-reactivity Ito H-31 to reduce the viscosity of the overall material after mixing and slow down the reaction speed, thereby prolonging the gel time and providing favorable conditions for the floating of resin color sand.

[0032] 4) The present application uses branched polyether / polyester polyol to modify diphenylmethane diisocyanate, and then blends with polymethylene polyphenyl isocyanate for modification, so as to increase the crosslinking density of polyurethane, so that the floor material has high hardness and compression strength, scratch resistance and other properties; at the same time, the viscosity of the overall material after mixing is reduced, which helps the resin color sand to quickly float to achieve the expected effect. DETAILED DESCRIPTION

[0033] In order to make the objects, technical solutions and advantages of the present application clearer, the technical solutions of the present application will be described in detail below. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of the present application.

[0034] Embodiment 1

[0035] A, component B, component C, component D of a solvent-free polyurethane floating colored sand self-leveling floor material, the proportioning by weight is as follows:

[0036] Component A:

[0037]

[0038]

[0039] Component B:

[0040] Sovermol 815 4 parts

[0041] Diphenyl methane diisocyanate 20 parts

[0042] Polymethylene polyphenyl isocyanate 40 parts

[0043] Component C:

[0044] White resin colored sand (300 microns) 27 parts

[0045] Black resin colored sand (300 microns) 3 parts

[0046] Component D:

[0047] Quartz sand (140-280 mesh) 30 parts

[0048] Mixing component A, component B, component C, component D uniformly according to the ratio of 1:0.6:0.5:0.5 to obtain a solvent-free polyurethane floating colored sand self-leveling floor material.

[0049] Embodiment 2

[0050] A, component B, component C, component D of a solvent-free polyurethane floating colored sand self-leveling floor material, the proportioning by weight is as follows:

[0051] Component A:

[0052]

[0053]

[0054] Component B:

[0055] Sovermol 750 4 parts

[0056] Diphenylmethane diisocyanate 18 parts

[0057] Polymethylene polyphenyl isocyanate 48 parts

[0058] Component C:

[0059] White resin color sand (400 microns) 12 parts

[0060] Light green resin color sand (400 microns) 18 parts

[0061] Component D:

[0062] Quartz sand (140-280 mesh) 30 parts

[0063] The components A, component B, component C are mixed uniformly according to the ratio of 1:0.7:0.5:0.5 to obtain a solvent-free polyurethane floating color sand self-leveling floor material.

[0064] Example 3:

[0065] A solvent-free polyurethane floating color sand self-leveling floor material component A, component B, component C, component D, the proportioning by weight parts is as follows:

[0066] Component A:

[0067]

[0068] Component B:

[0069] Sovermol 760 4 parts

[0070] Diphenylmethane diisocyanate 18 parts

[0071] Polymethylene polyphenyl isocyanate 45 parts

[0072] Component C:

[0073] White resin color sand (300 microns) 15 parts

[0074] Blue resin color sand (300 microns) 15 parts

[0075] Component D:

[0076] Quartz sand (100-240 mesh) 30 parts

[0077] The components A, component B, component C are mixed uniformly according to the ratio of 1:0.7:0.5:0.5 to obtain a solvent-free polyurethane floating color sand self-leveling floor material.

[0078] Example 4:

[0079] A, component B, component C, component D of a solvent-free polyurethane floating colored sand self-leveling floor material, the proportion of which is as follows:

[0080] Component A:

[0081]

[0082] Component B:

[0083] Sovermol 1092 4 parts

[0084] Diphenylmethyl diisocyanate 18 parts

[0085] Polymethylene polyphenyl isocyanate 45 parts

[0086] Component C:

[0087] White resin colored sand (300 microns) 12 parts

[0088] Orange resin colored sand (300 microns) 18 parts

[0089] Component D:

[0090] Quartz sand (100-240 mesh) 30 parts

[0091] Mix component A, component B, component C, component D in the ratio of 1.0:0.6:0.5:0.5 to obtain a solvent-free polyurethane floating colored sand self-leveling floor material.

[0092] The resin colored sand of component C in examples 1-4 can be arbitrarily matched in proportion according to the visual effect requirements.

[0093] Comparative example

[0094] Commercially available solvent-free polyurethane self-leveling floor material.

[0095] Specific construction method:

[0096] (I) Base surface treatment:

[0097] Use a dustless sander to polish and remove impurities, and clean thoroughly; cut the damaged and shelled areas neatly first, then repair them to be flush with the surrounding area using epoxy mortar; check the flatness of the overall base surface, use high-grinding and low-repair method to make the base surface difference comply with 2 meters ruler ± 2mm; clean thoroughly.

[0098] (II) Primer:

[0099] The capillary pores of the overall floor are closed by using epoxy primer, and attention should be paid to avoid material accumulation and missed coating.

[0100] (Three) Mortar:

[0101] The epoxy mortar material is used for the construction of the overall floor to increase the flatness of the floor, and attention should be paid to control the construction thickness. After curing, polish and clean.

[0102] (Four) Middle coating:

[0103] The overall floor is constructed by using a toothless trowel to scrape the middle coating material.

[0104] (Five) Surface coating:

[0105] The solvent-free polyurethane floating color sand self-leveling floor material of Examples 1-4 is proportionally prepared by using a serrated trowel to scrape, and then the defoaming roller is used to cross at least twice. Performance test:

[0106] According to GB / T 22374-2018, the performance of Examples 1-4 and the comparative example is tested, and the test results are shown in Table 1.

[0107] Table 1 is the performance test results of the floor materials of Examples 1-4 and the comparative example.

[0108]

[0109]

[0110] The floor material introduces branched polyether / polyester polyol modified diphenyl methane diisocyanate, and is blended with polymethylene polyphenyl isocyanate, increases the crosslinking density of polyurethane, makes the floor have high hardness and high compressive strength; at the same time, the single functional low viscosity H-31 reduces the viscosity of the overall material after mixing and slows down the reaction speed, which provides favorable conditions for the floating of color sand; and the addition of light PMMA resin color sand enriches the color of the solvent-free polyurethane self-leveling floor system, greatly improves the decoration, and significantly improves the pencil hardness (scratch resistance) of the polyurethane floor, which can reach 4-5H, which is difficult to achieve by ordinary polyurethane self-leveling floor; the floor wear resistance of the present application is only 4-10mg under the condition of 750g / 500r, which is equivalent to the high wear-resistant polyurethane material of patent CN106893380A, but at the same time has high decoration and high compressive strength.

[0111] The above merely describes specific embodiments of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the present application, which should be covered within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims. In addition, it should be noted that, in the above specific embodiments, various specific technical features can be combined in any appropriate manner without contradiction, in order to avoid unnecessary repetition, the present application will not further describe various possible combinations. Furthermore, various different embodiments of the present application can also be combined in any manner, as long as it does not violate the idea of the present application, it should also be considered as disclosed by the present application.

Claims

1. A solvent-free polyurethane floating colored sand self-leveling flooring material, characterized in that, It includes components A, B, C, and D; the mass ratio of each component is as follows: Component A: Component B: Component C: Component D = 1~1.5: 0.5~1: 0.3~0.6: 0.3~0.6; Component A, by weight, comprises the following materials: 20-30 parts by weight of branched polyether / polyester polyol, 10-20 parts by weight of refined castor oil, 5-10 parts by weight of modified castor oil, 0.2-0.5 parts by weight of wetting agent, 0.5-0.8 parts by weight of dispersant, 0.4-0.8 parts by weight of leveling agent, 0.3-0.6 parts by weight of defoamer, 8-12 parts by weight of dehydrating agent, 60-80 parts by weight of filler, and 2-4 parts by weight of pigment; Component B, by weight, comprises the following materials: 15-25 parts by weight of the modified branched polyether / polyester polyol p-diphenylmethane diisocyanate, and 30-50 parts by weight of polymethylene polyphenyl isocyanate. Component C, by weight, includes the following materials: 25-40 parts by weight of resin-floating colored sand; Component D, by weight, includes the following materials: 25-40 parts by weight of quartz sand. The branched polyether / polyester polyol in component A is BASF Sovermol. One or more of Sovermol 750, Sovermol 760, Sovermol 815, and Sovermol 1092, with a hydroxyl value of 200-400; refined castor oil with a hydroxyl value of 150-175; modified castor oil is Ito H-31 with a hydroxyl value of 157-170; the dehydrating agent is highly active nano-zeolite powder; the filler is one or more of 600-2000 mesh alumina, aluminum hydroxide, silica powder, calcium carbonate, and mineral barium sulfate; the dispersant is one or more of BYK-P104S, BYK-2151, BYK-163, BYK-9076, and BYK-9011; the wetting agent is one or more of BYK-349 and BYK-3455; the leveling agent is BYK-354; and the defoamer is one or more of BYK-054, BYK-066N, and BYK-1794. Component B requires the addition of branched polyether / polyester polyol to modify diphenylmethane diisocyanate to obtain a modified product, wherein the branched polyether / polyester polyol is one or more of Sovermol 750, Sovermol 760, Sovermol 815, and Sovermol 1092; the diphenylmethane diisocyanate is WANNATE MDI-50; and the polymethylene polyphenyl isocyanate is one or more of WANNATE PM-200 and WANNATE PM-400. The modified compound is prepared by mixing branched polyether / polyester polyol and diphenylmethane diisocyanate at a weight ratio of 1:4 to 10, heating to 70 to 90°C in a nitrogen-protected reactor, and stirring for 1 to 1.5 hours; after the reaction is completed, cooling is performed to obtain the modified compound. Component C is dry PMMA resin colored sand particles with a particle size of 200-400 micrometers and a density of 1.1-1.2 g / cm³. 3 ; Component D is dry 100-400 mesh quartz sand particles, or 140-280 mesh quartz sand particles.

2. The method for preparing the solvent-free polyurethane floating colored sand self-leveling flooring material according to claim 1, characterized in that, Includes the following steps: Step 1, Preparation of Group A Material: Branched polyether / polyester polyol, refined castor oil, modified castor oil, wetting agent, dispersant, dehydrating agent, filler, and pigment are added to a vacuum high-speed mixer according to the formula ratio. The mixture is stirred under vacuum at room temperature for at least 30 minutes. Then, leveling agent and defoamer are added, and the mixture is stirred under vacuum at room temperature for at least 30 minutes to remove bubbles. The mixture is then sealed and packaged to obtain Group A material. The filler should be pre-dried at 120°C for at least 1 hour to remove moisture, and used after cooling. Step 2, Preparation of Group B materials: Branched polyether / polyester polyol and diphenylmethane diisocyanate are mixed evenly at a weight ratio of 1:4 to 10. In a reaction vessel under nitrogen protection, the temperature is raised to 70 to 90°C and the mixture is stirred for 1 to 1.5 hours. After the reaction is completed, the mixture is cooled to obtain the modified material. Under stirring conditions, polymethylene polyphenyl isocyanate was added to the modified material according to the formula ratio and mixed for 0.5 h. The mixture was then sealed and packaged to obtain component B. Step 3, Preparation of Group C material: Dry-mix the selected color of dried PMMA resin colored sand and seal it to obtain Group C. Step 4, Preparation of Group D material: Dry quartz sand is sealed and packaged to obtain Group D; Step 5: When using, mechanically mix components A, B, C, and D in the weight ratio of component A: component B: component C: component D = 1~1.5: 0.5~1: 0.3~0.6: 0.3~0.6 to obtain a solvent-free polyurethane floating colored sand self-leveling flooring material.

Images