Composite material for super-wear-resistant dust-free workshop antiskid terrace and preparation process of composite material
By using composite materials containing bio-based resins and self-healing microcapsules, combined with layered construction technology, the problems of insufficient wear resistance, self-healing ability, and anti-slip performance of cleanroom flooring materials have been solved, achieving improvements in high wear resistance, long-lasting anti-slip performance, and environmental protection.
Patent Information
- Application Number
- CN202511012049.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-11-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Existing cleanroom flooring materials are inadequate in terms of wear resistance, self-healing ability, anti-slip performance, and environmental friendliness. Furthermore, traditional materials are prone to cracking during use, have high maintenance costs, and do not meet the requirements of green and sustainable development.
The composite material, consisting of bio-based resin, self-healing microcapsules, nano-reinforcement and interface modifiers, composite wear-resistant aggregates and high-hardness polymers, is used to form a floor with self-healing ability, long-lasting anti-slip performance and high wear resistance through layered construction technology. Environmentally friendly diluents and additives are used to reduce VOC emissions.
It significantly extends the service life of the flooring, improves its overall wear resistance, ensures long-lasting and effective anti-slip performance, and reduces environmental impact, meeting the requirements of green building.
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Figure CN120904752A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of high polymer composite materials, in particular to a super wear-resistant composite material for dust-free workshop anti-skid floor and a preparation process thereof. BACKGROUND
[0002] The requirements for floor materials in special industrial environments such as dust-free workshops, precision manufacturing, food and medicine are increasingly stringent. Not only do they need to have excellent wear resistance, impact resistance, dust prevention and easy cleaning basic physical properties, but they also have higher standards for safety, service life and green environmental protection. Although traditional epoxy resin floors and polyurethane floors are widely used, they often have some inherent defects during long-term use.
[0003] For example, these floor materials are prone to cracking when subjected to mechanical damage or temperature stress, and lack effective damage repair mechanisms, resulting in high maintenance costs and affecting production continuity. To improve wear resistance, hard fillers are often added, but the interface bonding between the fillers and the resin matrix often leads to poor durability of wear resistance. At the same time, the anti-skid performance of the floor usually depends on the surface structure or short-term coating, and it is difficult to maintain long-term effectiveness under continuous wear and tear. In addition, many traditional floor materials are not environmentally friendly during production and construction, and the emission of volatile organic compounds (VOC) and excessive dependence on petrochemical resources do not meet the current trend of green and sustainable development.
[0004] Therefore, the present application proposes a super wear-resistant composite material for dust-free workshop anti-skid floor and a preparation process thereof to solve the problems of the prior art. SUMMARY
[0005] In view of the deficiencies of the prior art, the present application provides a super wear-resistant composite material for dust-free workshop anti-skid floor and a preparation process thereof, which solves the problems of floor materials in terms of self-repairing ability, comprehensive durability, long-term anti-skid function and green environmental protection performance.
[0006] To achieve the above purpose, the present application realizes the following technical scheme: a super wear-resistant composite material for dust-free workshop anti-skid floor, comprising the following components by mass fraction:
[0007] Bio-based resin: 50-70 parts;
[0008] Self-repairing microcapsules: 5-15 parts;
[0009] Nano-enhanced and interface modifier: 1-5 parts;
[0010] Composite wear-resistant aggregate: 20-40 parts;
[0011] High-hardness polymer: 3-10 parts;
[0012] Bio-based curing agent: 50-70 parts;
[0013] Environment-friendly diluent and auxiliary agent: 2-15 parts.
[0014] Preferably, the bio-based resin is cashew phenol modified vegetable oil based epoxy resin or castor oil based polyurethane prepolymer; the bio-based curing agent is vegetable oil fatty acid modified amine curing agent or bio-based polyol or polyisocyanate chain extender which is chemically reacted with the bio-based resin.
[0015] The composite material takes bio-based resin as the main film-forming material, supplemented by bio-based curing agent. Specifically, the bio-based resin is selected from cashew phenol modified vegetable oil based epoxy resin or castor oil based polyurethane prepolymer. Both cashew phenol and vegetable oil are derived from renewable resources, which significantly improves the bio-based content of the material and conforms to the development trend of green environmental protection. The introduction of cashew phenol can improve the flexibility of traditional epoxy resin and endow the material with certain hydrophobicity and chemical resistance due to its unique benzene ring and long-chain aliphatic hydrocarbon structure. The castor oil based polyurethane prepolymer endows the material with good elasticity and impact resistance due to the flexible long chain contained in its molecular chain.
[0016] The matching bio-based curing agent, such as vegetable oil fatty acid modified amine curing agent or bio-based polyol or polyisocyanate chain extender, not only ensures the efficient chemical cross-linking reaction with the bio-based resin to form a dense and stable three-dimensional network structure, thereby guaranteeing the mechanical strength and durability of the material, but also further strengthens the bio-based characteristics and environmental protection properties of the whole system.
[0017] Preferably, the wall material of the self-repairing microcapsule is polyurea-formaldehyde or polyurethane, the core material thereof is a mixture containing epoxy resin repair agent and latent curing agent, or isocyanate repair agent, and the average particle size of the self-repairing microcapsule is 20-100 microns.
[0018] In order to prolong the service life of the floor material, self-repairing microcapsules are introduced. The wall material of these microcapsules is polyurea-formaldehyde or polyurethane, which has good mechanical strength and coating stability to the core material. The core material contains a mixture of epoxy resin repair agent and latent curing agent, or isocyanate repair agent. When the composite material is subjected to external force during use and produces microcracks, the expansion of the cracks will tear the self-repairing microcapsules passing through.
[0019] The repair agent (such as epoxy resin and curing agent, or isocyanate) in the capsule core will flow into the crack area by capillary action, and chemical reaction (such as epoxy ring-opening polymerization or isocyanate polymerization with moisture in the air or active hydrogen in the matrix) will occur, thereby "actively" repairing the crack, preventing further expansion of the crack, and restoring the mechanical properties of the material. The average particle size of 20-100 microns is designed to ensure that the microcapsules can be effectively dispersed in the floor material and release the repair agent in time and sufficient amount when the crack occurs, realizing efficient self-healing function.
[0020] Preferably, the nano-enhancing and interface-modifying agent is surface-functionalized nanosilica or surface-functionalized nanotube; and the composite wear-resistant aggregate comprises spherical ceramic microbeads and siliconized corundum particles.
[0021] To achieve the goal of "super wear resistance", the synergistic effect of nano-enhancing and interface-modifying agent and composite wear-resistant aggregate is adopted. The nano-enhancing and interface-modifying agent is surface-functionalized nanosilica or surface-functionalized nanotube. These nanomaterials can significantly improve the mechanical properties of the polymer matrix due to their large specific surface area and quantum size effect. More importantly, through surface functionalization treatment, the dispersibility of the nanofiller in the bio-based resin is improved, and the interfacial bonding strength between the nanofiller and the resin matrix is enhanced. This not only effectively transmits stress and prevents the initiation and propagation of microcracks, but also improves the hardness and scratch resistance of the material.
[0022] The composite wear-resistant aggregate comprises spherical ceramic microbeads and siliconized corundum particles. Spherical ceramic microbeads have high hardness, low density and good chemical stability, and can effectively resist wear. Corundum particles themselves have extremely high hardness and are excellent wear-resistant fillers. Through surface silanization treatment, a "molecular bridge" is built between the inorganic filler and the organic resin matrix using silane coupling agent, greatly improving the compatibility and bonding force of the two-phase interface, so that the corundum particles can be more firmly anchored in the resin matrix, avoiding falling off under high stress and wear conditions, and thus fully exerting their wear resistance performance.
[0023] Preferably, the high-hardness polymer is a micrometer-sized particle or short fiber with regular or semi-regular geometric shape, and the micrometer-sized particle or short fiber is selected from a composite material of polymethyl methacrylate and ceramic powder or glass fiber reinforced epoxy resin short fibers; the environmentally friendly diluent and auxiliary agent comprises an active diluent selected from cardanol glycidyl ether or epoxidized soybean oil, a leveling agent selected from polyether modified polysiloxane leveling agent, a defoaming agent selected from mineral oil-based or silicone-based defoaming agent, and a wetting dispersant selected from a high molecular dispersant with acidic groups.
[0024] The anti-slip performance of the floor is provided by high-hardness polymers. These polymers are in the form of micron-sized particles or short fibers with regular or semi-regular geometric shapes, and are made of composite materials of polymethyl methacrylate and ceramic powder or short fibers of glass fiber reinforced epoxy resin. These microstructures are partially exposed or slightly protruding from the surface of the floor after the curing of the topcoat, forming regular or semi-regular rough peaks, which achieve the anti-slip effect by increasing the friction coefficient between the floor and the contacting objects (such as shoe soles and tires). The micron-sized size and specific geometric shape help to form effective and durable anti-slip textures, while the selection of high-hardness composite materials ensures the wear resistance of the anti-slip structures themselves.
[0025] Active diluents such as cardanol glycidyl ether or epoxidized soybean oil not only effectively reduce the viscosity of the system, making it easy to apply, but also contain functional groups that can participate in the curing reaction, becoming part of the cured product, thereby reducing the emission of volatile organic compounds (VOC). Leveling agents (such as polyether-modified polysiloxanes) ensure that the coating surface is smooth and flat, defoamers (such as mineral oil-based or silicone-based) eliminate bubbles generated during application, and wetting dispersants (such as high molecular weight dispersants with acidic groups) ensure uniform and stable dispersion of various fillers in the resin. The synergistic effect of these additives ensures that the floor coating has good application performance and final coating quality, while meeting environmental protection requirements.
[0026] The application also provides a preparation process for a super-wear-resistant dust-free workshop anti-slip floor composite material, including the following steps:
[0027] S1, base surface pretreatment, including cleaning, leveling, mechanical polishing or shot blasting treatment of the concrete base surface, and ensuring that the base surface is dry;
[0028] S2, preparation of a bio-based penetration-enhancing primer layer, including mixing the bio-based resin, the bio-based curing agent, and the diluent and additives in the environmentally friendly diluent, and then applying the mixture to the pretreated base surface and preliminary curing;
[0029] S3, preparation of a bio-based self-repairing wear-resistant intermediate coating, including uniformly mixing the bio-based resin, self-repairing microcapsules, nano-enhancing and interface modifying agents, composite wear-resistant aggregates, bio-based curing agents, and environmentally friendly diluents and additives, then spreading the mixture on the primer layer and curing to form an intermediate coating containing self-repairing microcapsules and composite wear-resistant aggregates;
[0030] S4, preparation of a long-acting anti-slip functional topcoat, including uniformly mixing the bio-based resin, nano-enhancing and interface modifying agents, bio-based curing agents, and environmentally friendly diluents and additives to form a topcoat slurry, applying the topcoat slurry to the intermediate coating, and then implanting high-hardness polymers before the topcoat slurry is completely cured.
[0031] Preferably, in the S1 step, the concrete base surface is cleaned to remove oil stains, floating slurry, old coatings and loose materials, and is leveled;
[0032] The cleaned and leveled concrete base surface is then mechanically polished or shot blasted to form a CSP 3-5 grade surface roughness profile;
[0033] And before applying the bio-based permeability enhancement primer, the moisture content of the base surface is ensured to be less than 5.0%.
[0034] Preferably, in the S2 step, the bio-based permeability enhancement primer is applied in an amount of 0.15-0.25 kg / m 2 , and the initial curing is carried out at an ambient temperature of 20-25°C for 4-8h until it reaches a tack-free state.
[0035] Preferably, in the S3 step, the bio-based self-repairing wear-resistant intermediate coating is applied with a thickness of 2.0-4.0mm, and immediately after application, a defoaming roller is used to eliminate air bubbles, and then it is cured at an ambient temperature of 20-25°C for 12-24h until it reaches a recoatable state.
[0036] Preferably, in the S4 step, the bio-based resin, the nano-enhancing and interface modifier, the bio-based curing agent and the environmentally friendly diluent and auxiliary agents are uniformly mixed to form a topcoat slurry, which is uniformly applied to the intermediate coating using a roller or blade coating method, and the wet film thickness is controlled to be 0.1-0.3mm;
[0037] Before the topcoat slurry reaches a tack-free state, the high-hardness polymer is uniformly implanted into the surface layer of the topcoat slurry by precision spreading or electrostatic sanding, and the spreading amount is 100-300g / m 2 ;
[0038] Then it is cured at an ambient temperature of 20-25°C for 24-48h to form the long-acting anti-slip functional topcoat.
[0039] The present application provides a kind of super wear-resistant dust-free workshop anti-slip floor with composite material and its preparation process.It has the following beneficial effects:
[0040] 1、The present application constructs a new type of floor composite material by the synergistic effect of specific bio-based resin, self-repairing microcapsule and composite wear-resistant aggregate.It gives the floor the ability to actively repair when damaged by microcracks, significantly prolonging the service life.Compared with traditional floor materials that need to be repaired manually or replaced as a whole once cracked, the present application effectively overcomes the problem of passive response to damage and high maintenance cost.
[0041] 2、The floor material of the present application obtains excellent comprehensive wear resistance by introducing nano-enhancing agents into the bio-based main material and optimizing the interface bonding with multi-scale wear-resistant aggregates. Compared with the previous technology that simply relies on high-hardness aggregate accumulation to improve wear resistance but is prone to aggregate shedding due to poor interface bonding, the present application solves the problems of insufficient wear resistance durability and rapid performance degradation.
[0042] 3、The present application adopts a layered functional construction strategy, especially by precisely controlling the specific surface roughness formed by base surface pretreatment and applying a homologous bio-based penetration-enhancing primer. This method ensures the formation of a firm physical and chemical double anchoring between the floor system and the concrete base material. This changes the traditional floor construction, which only focuses on surface cleaning and ignores the construction of interface microstructure, thereby causing the problems of insufficient adhesion and easy hollowing and delamination.
[0043] 4、In the preparation of the topcoat layer, the present application uses a precise implantation technology of high-hardness polymer particles instead of simple mixing and coating. This surface construction method forms a durable and effective anti-skid texture on the floor surface. Compared with the technology that relies on the friction coefficient of the coating itself or short-term surface treatment to obtain anti-skid effect, the present solution overcomes the limitation that the anti-skid performance quickly decreases with use and wear.
[0044] 5、The present application as a whole uses a high bio-based content main material and an environmentally friendly additive system, significantly reducing the dependence on petrochemical resources and volatile organic compound emissions during construction. Compared with traditional epoxy and polyurethane floor materials that use a large amount of solvent or have high VOC content, the present solution solves the pain points of high environmental load and non-compliance with green building requirements while ensuring high performance. BRIEF DESCRIPTION OF DRAWINGS
[0045] Figure 1 The flowchart of the method of the present application. DETAILED DESCRIPTION
[0046] The technical solutions in the embodiments of the present application will be described below in conjunction with the drawings of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.
[0047] Please refer to Figure 1 :
[0048] The raw materials and reagents used in the following examples are commercially available or can be prepared by known methods.
[0049] Example 1:
[0050] Combination formula (mass fraction): Bio-based resin: 60 parts; Self-repairing microcapsule: 10 parts; Nano-enhanced and interface modifier: 3 parts; Composite wear-resistant aggregate: 30 parts; High-hardness polymer: 6 parts; Bio-based curing agent: 60 parts; Environment-friendly diluent and auxiliary agent: 8 parts.
[0051] Preparation process:
[0052] S1: Base surface pretreatment: Select the concrete base surface, first clean thoroughly, remove surface oil, slurry, old coating and loose material. Leveling treatment is carried out on uneven places. Then, the cleaned and leveled concrete base surface is treated by mechanical grinding until a CSP4 level surface roughness profile is formed. Before the next step of construction, use a humidity detector to detect and ensure that the base surface moisture content is controlled below 3.5%.
[0053] S2: Preparation of bio-based penetration-enhanced primer coating: Mix 60 parts of the bio-based resin, 60 parts of the bio-based curing agent, and an appropriate amount of active diluent (for example, 2 parts of cashew phenol glycidyl ether, and the remaining auxiliary agents are added as needed and deducted from the total auxiliary agent fraction) in the stirring container to form a low-viscosity primer. The primer is evenly applied to the pretreated base surface, and the coating amount is controlled at 0.20 kg / m 2 . Curing at ambient temperature 22.5℃ for 6h until the primer reaches a tack-free state.
[0054] S3: Preparation of bio-based self-repairing wear-resistant intermediate coating: Mix 60 parts of the bio-based resin, 10 parts of the self-repairing microcapsule, 3 parts of the nano-enhanced and interface modifier, 30 parts of the composite wear-resistant aggregate, 60 parts of the bio-based curing agent, and the remaining environment-friendly diluent and auxiliary agent (for example, 6 parts, including leveling agent, defoaming agent, dispersant, etc.) in the stirring equipment to form an intermediate coating slurry. The slurry is evenly spread on the tack-free primer, and the spreading thickness is controlled at 3.0mm. After spreading, immediately use a defoaming roller to roll back and forth on the surface of the intermediate coating to eliminate the air bubbles generated during construction. Then, curing at ambient temperature 22.5℃ for 18h until the intermediate coating reaches a coatable state.
[0055] S4: Preparation of long-lasting anti-slip functional topcoat: 60 parts of the bio-based resin, 3 parts of the nano-enhancing and interface modifying agent, 60 parts of the bio-based curing agent, and appropriate amount of the environmentally friendly diluent and auxiliary agent (to ensure good workability, for example, 4 parts, allocated from the total auxiliary agent parts) are uniformly mixed to form a topcoat slurry. The topcoat slurry is uniformly coated on the surface of the cured midcoat layer using a roll coating method, with the wet film thickness controlled at 0.2 mm. Before the topcoat slurry reaches the tack-free state (usually within 30-60 minutes after coating, depending on the environmental temperature and humidity), 6 parts of the high-hardness polymer particles are uniformly spread on the surface of the wet topcoat slurry using a precision spreading device, with the spreading amount controlled at 200 g / m 2 . After the spreading is completed, the coating is naturally cured at an ambient temperature of 22.5°C for 36 h to form an ultra-wear-resistant floor with long-lasting anti-slip function.
[0056] Example 2:
[0057] Combined formulation (mass parts): bio-based resin: 50 parts; self-repairing microcapsule: 5 parts; nano-enhancing and interface modifying agent: 1 part; composite wear-resistant aggregate: 20 parts; high-hardness polymer: 3 parts; bio-based curing agent: 50 parts; environmentally friendly diluent and auxiliary agent: 2 parts.
[0058] Preparation process:
[0059] S1: Base surface pretreatment: clean and level the concrete base surface. Use shot blasting treatment to process the base surface to form a CSP3-level surface roughness profile. Ensure that the water content of the base surface is less than 5.0% (for example, the detected value is 4.8%).
[0060] S2: Preparation of bio-based penetration-enhancing primer coat: 50 parts of the bio-based resin, 50 parts of the bio-based curing agent, and appropriate amount of the active diluent in the environmentally friendly diluent and auxiliary agent are mixed, and then applied to the base surface at a coating amount of 0.15 kg / m 2 . Cured at an ambient temperature of 20°C for 4 h to tack-free.
[0061] S3: Preparation of bio-based self-repairing wear-resistant midcoat: 50 parts of the bio-based resin, 5 parts of the self-repairing microcapsule, 1 part of the nano-enhancing and interface modifying agent, 20 parts of the composite wear-resistant aggregate, 50 parts of the bio-based curing agent, and the remaining environmentally friendly diluent and auxiliary agent are uniformly mixed and spread on the primer coat to a thickness of 2.0 mm. Immediately treated with a defoaming roller. Cured at an ambient temperature of 20°C for 12 h.
[0062] S4: Preparation of long-acting anti-skid functional topcoat: 70 parts of the bio-based resin, 5 parts of the nano-enhancing and interface modifier, 70 parts of the bio-based curing agent and appropriate amount of environmentally friendly diluent and auxiliary were mixed to form a topcoat slurry, which was roll-coated on the middle coating layer, and the wet film thickness was controlled to be 0.3 mm. Before the surface drying of the topcoat slurry, 10 parts of the high-hardness polymer was implanted by electrostatic sanding, and the sanding amount was 300 g / m 2 . Curing at ambient temperature 20℃ for 24h.
[0063] Example 3:
[0064] Combined formula (mass fraction): bio-based resin: 70 parts; self-repairing microcapsule: 15 parts; nano-enhancing and interface modifier: 5 parts; composite wear-resistant aggregate: 40 parts; high-hardness polymer: 10 parts; bio-based curing agent: 70 parts; environmentally friendly diluent and auxiliary: 15 parts.
[0065] Preparation process:
[0066] S1: Base surface pretreatment: clean and level the concrete base surface. The base surface is treated by mechanical grinding to form a CSP5 level surface roughness profile. Ensure that the water content of the base surface is less than 5.0% (for example, the test value is 2.0%).
[0067] S2: Preparation of bio-based penetration-enhancing primer coating: 70 parts of the bio-based resin, 70 parts of the bio-based curing agent and appropriate amount of active diluent in the environmentally friendly diluent and auxiliary are mixed, and then applied to the base surface at a coating amount of 0.25 kg / m 2 . Curing at ambient temperature 25℃ for 8h to surface dry.
[0068] S3: Preparation of bio-based self-repairing wear-resistant middle coating: 70 parts of the bio-based resin, 15 parts of the self-repairing microcapsule, 5 parts of the nano-enhancing and interface modifier, 40 parts of the composite wear-resistant aggregate, 70 parts of the bio-based curing agent and the remaining environmentally friendly diluent and auxiliary are uniformly mixed and spread on the primer coating, and the thickness is controlled to be 4.0 mm. Immediately use a defoaming roller to process. Curing at ambient temperature 25℃ for 24h.
[0069] S4: Preparation of long-acting anti-skid functional topcoat: 70 parts of the bio-based resin, 5 parts of the nano-enhancing and interface modifier, 70 parts of the bio-based curing agent and appropriate amount of environmentally friendly diluent and auxiliary were mixed to form a topcoat slurry, which was roll-coated on the middle coating layer, and the wet film thickness was controlled to be 0.3 mm. Before the surface drying of the topcoat slurry, 10 parts of the high-hardness polymer was implanted by electrostatic sanding, and the sanding amount was 300 g / m 2 . Curing at ambient temperature 25℃ for 48h.
[0070] Comparative Example 1:
[0071] The difference compared with Example 1 is that the self-repairing microcapsules are not contained in the combined formulation, and the mass fraction is replaced by the bio-based resin (cashew modified vegetable oil based epoxy resin) in the same proportion, that is, the amount of bio-based resin is increased to 70 parts. The self-repairing microcapsules are not added in the S3 step of the preparation process. The remaining components, proportions and preparation process steps are the same as Example 1.
[0072] Comparative Example 2:
[0073] The difference compared with Example 1 is that the nano-enhanced and interface modifier (surface functionalized nano-silicon dioxide) is not contained in the combined formulation, and the mass fraction is replaced by the composite wear-resistant aggregate in the same proportion, that is, the amount of composite wear-resistant aggregate is increased to 33 parts. The nano-enhanced and interface modifier is not added in the S3 and S4 steps of the preparation process. The remaining components, proportions and preparation process steps are the same as Example 1.
[0074] Comparative Example 3:
[0075] The difference compared with Example 1 is that the composite wear-resistant aggregate in the combined formulation only uses corundum particles without surface silane treatment, instead of the original formula “contains spherical ceramic microbeads and corundum particles with surface silane treatment”, the total mass fraction is still 30 parts. The remaining components, proportions and preparation process steps are the same as Example 1.
[0076] Comparative Example 4:
[0077] The difference compared with Example 1 is that the mass fraction of high-hardness polymer in the combined formulation is 15 parts. The remaining components, proportions and preparation process steps are the same as Example 1.
[0078] Comparative Example 5:
[0079] The difference compared with Example 1 is that the mechanical polishing or shot blasting step in the S1 base surface pretreatment step of the preparation process is omitted, only cleaning and leveling treatment is performed, and the surface roughness profile of CSP3-5 grade is not required. The remaining components, proportions and preparation process steps are the same as Example 1.
[0080] Comparative Example 6:
[0081] The difference compared with Example 1 is that in the S4 long-acting anti-skid functional topcoat preparation step of the preparation process, the high-hardness polymer is mixed uniformly with other components (bio-based resin, nano-enhanced and interface modifier, bio-based curing agent, environmentally friendly diluent and auxiliary agent) of the topcoat slurry, and then directly roller coated on the midcoat, instead of being implanted before the topcoat slurry is completely cured. The remaining components, proportions and preparation process steps are the same as Example 1.
[0082] Test Example 1: Comparison of Material Core Mechanics and Durability Performance
[0083] Scratch repair ability evaluation:
[0084] Test objects: samples prepared according to Example 1 (denoted as S-E1); samples prepared according to Comparative Example 1 (denoted as S-C1); 3 parallel samples of each sample type, with a size of 100 mm x 100 mm x 5 mm.
[0085] Main instruments and tools:
[0086] Adjustable load scratch tester (or simple scratch needle device, ensuring consistent scratch needle tip and controllable load); scratch needle: hard alloy steel needle, tip curvature radius 0.5 mm; digital camera or mobile phone with macro function; constant temperature and humidity chamber (environmental temperature controlled at 23 ± 2°C, relative humidity 50 ± 5%); ruler;
[0087] Experimental steps are as follows:
[0088] Sample curing and humidity adjustment: after preparation, all samples are placed in a constant temperature and humidity chamber for at least 7 days to ensure complete curing and reach equilibrium state.
[0089] Scratch preparation: remove the sample, and on the smooth test surface of each sample, use the scratch tester (or simple scratch needle device) to apply a vertical load of 5 N (Newton), and draw a straight line scratch with a length of 30 mm at a speed of 10 mm / s. Ensure that the scratch conditions on each sample are consistent. Immediately take a photo of the newly generated scratch using a digital camera (fixed shooting distance and angle), and use a ruler to roughly measure the initial apparent width of the scratch (for example, use a camera with macro function to estimate the width, or use a high-precision reading microscope for preliminary observation, but do not perform microscopic structure analysis).
[0090] Repair process observation and recording: immediately place the scratched sample back into the constant temperature and humidity chamber. Remove the sample at 24 hours and 48 hours after scratch generation. Take a photo of the scratch area under the same shooting conditions. Visually assess the healing of the scratch, and describe whether the scratch edge is blurred, the scratch depth is shallower, and the scratch as a whole is less obvious. The remaining apparent width of the scratch can be roughly measured.
[0091] Data compilation: compile the photos and observation records.
[0092] Wear resistance test (Taber abrasion method):
[0093] Test samples: samples prepared according to Example 1 (denoted as A-E1); samples prepared according to Comparative Example 2 (denoted as A-C2); samples prepared according to Comparative Example 3 (denoted as A-C3); 3 round or square coupons (e.g. 100 mm in diameter, with a hole in the center, about 5 mm in thickness) for each sample were prepared according to the requirements of Taber Abrader.
[0094] Main instruments and tools:
[0095] Taber Abrader; Abrasive wheel type: CS-10 (or H series abrasive wheel according to the actual material properties); Additional load: 500 g per arm (or selected according to the standard, e.g. 1000 g in total); Analytical balance (accuracy 0.1 mg); Dust collection device (for cleaning the abrasion debris); Constant temperature and humidity chamber;
[0096] Experimental procedure:
[0097] Sample curing and humidity conditioning: all samples were placed in the constant temperature and humidity chamber for at least 7 days after preparation and were subjected to humidity conditioning until the constant weight.
[0098] Initial mass measurement: the initial mass of the sample after humidity conditioning was measured on the analytical balance to an accuracy of 0.1 mg and recorded as M0.
[0099] Abrasion test:
[0100] The sample was installed on the turntable of the Taber Abrader.
[0101] The appropriate abrasive wheel (e.g. CS-10) was selected and the specified additional load (e.g. 500 g per arm) was installed.
[0102] The abrasion rotation number was set to 1000 (or adjusted according to the abrasion resistance of the material to ensure a measurable amount of wear).
[0103] The abrasion tester was started, and the dust collection device was turned on.
[0104] Post-abrasion mass measurement:
[0105] After reaching the preset rotation number, the sample was removed.
[0106] The sample surface was gently cleaned of abrasion debris using a soft brush or a dust collection device.
[0107] The post-abrasion mass of the sample was measured again on the analytical balance to an accuracy of 0.1 mg and recorded as M1.
[0108] Mass loss calculation: the mass loss AM = M0-M1 was calculated.
[0109] Data processing: the abrasion mass loss of each sample was recorded.
[0110] Experimental data as shown in Table 1-2:
[0111] Table 1: Evaluation of scratch repair capability of different plaques
[0112]
[0113]
[0114] Table 2: Taber abrasion performance test results of different plaques (CS-10 abrasive wheel, 500g / arm, 1000 revolutions)
[0115]
[0116]
[0117] Summary of experiments:
[0118] By observing the scratch repair capability of different formulations, it was found that the composite containing specific microcapsules (e.g. S-E1 plaque) showed a significant decrease in the apparent width of the scratch over time, almost returning to a smooth state visually. This is attributed to the pre-installed self-repairing microcapsules that can rupture under external force and release their internal repair agents when the material generates micro-cracks. These repair agents then undergo chemical reactions and solidify in the crack area, filling and repairing the damage, giving the material an intelligent self-maintenance feature, which is significantly different from the materials without such microcapsules (e.g. S-C1 plaque) that show persistent scratches.
[0119] In terms of wear resistance, the composite with complete component design and containing nano-enhancing and interfacial modifiers (e.g. A-E1 plaque) showed the lowest mass loss in the Taber abrasion test. This is mainly because the nano-enhancing agent, such as surface-functionalized nano-silica, can effectively disperse in the bio-based resin matrix, significantly improving the mechanical strength and toughness of the matrix through its large specific surface area and optimized interfacial bonding, thereby enhancing the material's ability to resist abrasive wear. In contrast, the material lacking such nano-scale enhancement (e.g. A-C2 plaque) showed higher abrasion loss, indicating that it is more prone to material loss under friction and scratching.
[0120] Further abrasion comparison experiments reveal the importance of component synergy and interface treatment in the composite wear-resistant aggregate. Composite materials containing diamond particles treated with surface silane and spherical ceramic microbeads (such as A-E1 sample) exhibit better wear resistance, i.e. lower mass loss, compared to materials using only untreated diamond particles (such as A-C3 sample). The mechanism is that the surface modification of diamond particles by silane coupling agent forms an effective chemical bridge between inorganic fillers and organic resin matrix, greatly enhancing the bonding strength of the two-phase interface. This strong interface bonding makes the high-hardness diamond particles more firmly anchored in the resin matrix and less likely to be stripped during wear, thereby synergizing with other aggregate components such as spherical ceramic microbeads to improve the overall wear resistance of the material.
[0121] Test Example 2: Comparison of floor surface functionality and construction adaptability
[0122] Anti-slip performance test (pendulum friction coefficient measurement):
[0123] Test objects: sample prepared according to Example 1 (denoted as F-E1); sample prepared according to Comparative Example 4 (denoted as F-C4); sample prepared according to Comparative Example 6 (denoted as F-C6); prepare 3 flat samples of each sample, with a size of at least 300mm x 300mm and a thickness of about 5mm to meet the test requirements of the pendulum friction tester.
[0124] Main instruments and tools:
[0125] Pendulum friction coefficient tester (e.g. in accordance with GB / T-3903.33 or similar ASTM-E303 standard); standard rubber slider (selected according to test standards, such as TRL rubber slider); water spray pot (for wet state testing); thermometer; constant temperature and humidity chamber;
[0126] The experimental steps are as follows:
[0127] Sample curing and humidity adjustment: after preparation, all samples are placed in a constant temperature and humidity chamber for at least 7 days to ensure complete curing and reach equilibrium state (e.g. 23±2℃, relative humidity 50±5%).
[0128] Instrument calibration and preparation:
[0129] Calibrate the pendulum friction coefficient tester according to the instrument manual.
[0130] Ensure that the rubber slider is clean and meets the use requirements.
[0131] Record the test environment temperature.
[0132] Dry state anti-slip performance test:
[0133] Place the template horizontally and secure it on the base of the tester.
[0134] Release the pendulum and let the rubber slider on it slide over the surface of the template for the specified length.
[0135] Read the pendulum number (BPN) indicated by the pendulum pointer on the dial.
[0136] Take at least 5 measurements at different locations on each template and average the results. For the F-C4 template, pay particular attention to any differences in readings that can be caused by uneven distribution of the high hardness polymer.
[0137] Wet slip resistance test:
[0138] Spray a uniform layer of clean water over the test area on the template.
[0139] Repeat step 3 to measure the pendulum number under wet conditions.
[0140] Take at least 5 measurements at different locations on each template and average the results.
[0141] Data analysis: Record the average BPN values for each template under dry and wet conditions.
[0142] Observation of workability and surface condition (mainly for Comparative Example 4):
[0143] Test object: The process of preparing Comparative Example 4 (the process of preparing F-C4); compared with the S4 step of Example 1 (preparation of long-lasting slip-resistant functional topcoat).
[0144] Observation content and method:
[0145] Observation of topcoat slurry mixing (for F-C4): When preparing the topcoat slurry of Comparative Example 4, i.e. when the amount of high hardness polymer is 15 parts, observe the state of mixing with other components such as bio-based resin and curing agent. Record whether it is easy to mix evenly, whether there are phenomena such as polymer particle agglomeration, rapid sedimentation, or abnormal increase in slurry viscosity.
[0146] Observation of coating workability (for F-C4): When the topcoat slurry containing an excess amount of high hardness polymer is roll-coated on the midcoat, observe its leveling property, whether it is easy to form a uniform thickness of coating film, and whether the high hardness polymer particles are prone to dragging, piling up, or uneven distribution during the coating process.
[0147] Observation of surface state after curing (for F-C4): After the topcoat of the comparative example 4 sample was completely cured, the surface was visually inspected. The uniformity of the distribution of high-hardness polymer particles was observed, and whether there were phenomena of excessive exposure of particles, excessive embedding of particles, or lack / concentration of particles in local areas. The surface formed by the sanding process of the example 1 sample (F-E1) was compared.
[0148] The experimental data are shown in Table 3:
[0149]
[0150]
[0151] Table 4: Observations of workability and surface state (mainly for comparison between F-C4 and F-E1)
[0152]
[0153] Summary of the experiment:
[0154] The slip resistance of the floor surface is closely related to the introduction method and amount of the high-hardness polymer. The experimental results show that the sample (such as F-E1) in which the high-hardness polymer is embedded in the surface layer of the topcoat slurry by a specific embedding process exhibits a high surface friction coefficient (BPN value) under both dry and wet conditions. The mechanism is that the embedding process can anchor part of the high-hardness polymer particles in the topcoat, and at the same time, the particles are moderately protruding from the surface of the coating, forming a micro-rough, multi-point contact friction interface, thereby effectively increasing the friction force with the contacting object. In comparison, if the high-hardness polymer is directly mixed with the topcoat slurry and then applied (such as the F-C6 sample), the particles are easily completely covered by the resin, and it is difficult to form effective anti-slip protrusions, resulting in a significant reduction in the surface friction coefficient.
[0155] At the same time, the addition amount of the high-hardness polymer also has a significant influence on the workability and the final slip resistance. When the amount of the high-hardness polymer exceeds the appropriate range (such as the F-C4 sample), not only can there be problems such as inconvenient operation, uneven distribution of particles, and reduction of coating flatness during the mixing and application of the topcoat slurry, but also the final surface formed can be unstable due to particle accumulation or sparse distribution, resulting in a suboptimal or even reduced slip resistance. This shows that by accurately controlling the addition amount of the high-hardness polymer, a uniform and effective anti-slip structure can be formed in the topcoat, avoiding the construction difficulties or functional defects caused by improper addition amount, and achieving a good balance between material performance and process feasibility.
[0156] In summary, the floor material of the present application can achieve excellent surface anti-skid function, the key of which lies in the fine control of the preparation process of long-acting anti-skid functional surface coating and the optimization of the specific component dosage. By uniformly implanting an appropriate amount of high-hardness polymer into the surface coating slurry in a precise way such as precision scattering or electrostatic sanding when the surface coating slurry reaches a specific state, instead of simple mixing, the functional particles can form persistent and efficient anti-skid texture on the surface of the coating. The synergistic effect of the material composition and the preparation process ensures that the floor surface has good construction adaptability and provides reliable safety anti-skid protection.
[0157] Test Example 3: Comparison of the influence of key steps in the preparation process on the final adhesion performance
[0158] Coating adhesion test (pull-off method):
[0159] Test object: On the concrete substrate treated according to the S1 step (including mechanical polishing to form a CSP4 level surface roughness, and the water content of the base surface is controlled below 3.5%) in Example 1, continue to prepare a complete floor coating system according to the S2, S3, S4 steps of Example 1, and mark it as AD-E1.
[0160] On the concrete substrate treated according to the S1 step (only cleaning and leveling, omitting mechanical polishing or shot blasting treatment, and not specifically requiring CSP level surface roughness, assuming that the water content of the base surface is also controlled below 3.5% to exclude the interference of this variable) in Comparative Example 5, continue to prepare a complete floor coating system according to the S2, S3, S4 steps of Example 1, and mark it as AD-C5.
[0161] Prepare at least 3 concrete substrates of about 150mm x 150mm in size for each treatment. After preparing the floor coating on each substrate, select at least 3 test points for adhesion testing.
[0162] Main instruments and tools:
[0163] Pull-off adhesion tester (e.g. Elcometer-510, PosiTest-AT-A, or similar instruments conforming to ASTM-D4541 / ISO-4624 standards); standard diameter test stub (Dolly / Pull-stub, e.g. diameter 20mm); special adhesive (e.g. two-component epoxy adhesive, ensuring that its bonding strength is higher than the expected coating adhesion or cohesive strength); cutting tool (if necessary, cut the coating around the test stub to isolate the test area, according to the instrument requirements); constant temperature and humidity chamber (for curing of the sample and adhesive); cleaning supplies (such as solvents, for cleaning the test stub and coating surface);
[0164] Experimental steps:
[0165] Floor coating preparation and curing:
[0166] Prepare a complete floor coating system on two different pre-treated concrete substrates (AD-E1 substrate and AD-C5 substrate) according to the above instructions.
[0167] Cure the prepared floor panels in a constant temperature and humidity chamber (e.g., 23 ± 2°C, 50 ± 5% relative humidity) for at least 7 days.
[0168] Test anchor adhesion:
[0169] Select a flat, defect-free area of the coating surface as the test point.
[0170] Clean the test anchor bonding surface and the selected area of the coating surface with an appropriate solvent to ensure no oil or dirt.
[0171] Mix the two-component epoxy adhesive according to the manufacturer's instructions.
[0172] Apply a uniform, appropriate amount of adhesive to the bonding surface of the test anchor.
[0173] Press the adhesive-coated test anchor vertically onto the selected area of the coating surface, apply light pressure to remove air bubbles, and remove excess adhesive around the perimeter. Ensure good contact between the test anchor and the coating surface.
[0174] Allow the adhesive to cure under the specified conditions (e.g., room temperature or constant temperature and humidity chamber) according to the manufacturer's requirements (usually at least 24 hours, or as specified by the manufacturer).
[0175] Coating cutting: If required by the standard or instrument, after the adhesive has cured, use a specialized cutting tool to cut the coating around the edges of the test anchor to the substrate depth to ensure that the test force only acts on the coating area below the test anchor.
[0176] Adhesion testing: Connect the pull head of the pull-off adhesion tester to the cured test anchor correctly; ensure that the tester is perpendicular to the coating surface; apply a uniform pulling force at the loading rate set by the instrument (e.g., usually 0.2 MPa / s to 1.0 MPa / s in ASTM-D4541, or as selected according to the standard) until failure occurs (coating and substrate separation, internal coating failure, or adhesive failure); record the maximum pulling force value at the time of failure (usually the instrument will automatically convert it to pull-off strength, with units of MPa or psi).
[0177] Carefully observe and record the failure mode / interface:
[0178] A: Cohesive failure of the substrate (concrete failure); A / B: Interfacial failure of the primer to the substrate; B: Cohesive failure of the primer; B / C: Interfacial failure of the primer to the midcoat; C: Cohesive failure of the midcoat; C / D: Interfacial failure of the midcoat to the topcoat; D: Cohesive failure of the topcoat; Y: Interfacial failure of the adhesive to the topcoat (adhesive failure); Y / Z: Interfacial failure of the adhesive to the test anchor (adhesive failure); Z: Failure of the test anchor itself;
[0179] Data Compilation: The data from multiple test points on each panel were compiled, the average pull-off strength was calculated, and the failure mode was summarized.
[0180] Experimental data is shown in Table 5:
[0181] Table 5: Results of adhesion testing for floor coating systems on different substrate surface preparation
[0182]
[0183]
[0184] Experimental Summary:
[0185] The adhesion performance between the floor coating system and the concrete substrate is directly influenced by the substrate preparation process. The experimental results clearly show that after the concrete substrate is prepared by a process including mechanical grinding or shot blasting to form a specific surface roughness profile (such as the process adopted by the AD-E1 panel), the floor coating system prepared thereon exhibits significantly higher pull-off strength, and the failure mode mostly occurs within the concrete substrate or in the shallow layer where the coating and substrate are closely combined. This fully demonstrates the key role of the optimization of the substrate physical morphology in improving adhesion.
[0186] The core mechanism lies in that through mechanical grinding or shot blasting, not only are the floating slurry, weakly bonded layers and other substances that are not conducive to adhesion removed from the concrete surface, but more importantly, a large number of micro concave-convex structures are created on the substrate surface, i.e., a surface roughness profile with a specific grade is formed. This increased specific surface area and rich pore structure provides more superior mechanical locking points for the subsequent application of the bio-based penetration-enhancing primer. The primer can penetrate more deeply and extensively into these microstructures, and after curing, forms interlocking mechanical engagement, thereby greatly enhancing the physical bonding force between the coating and the substrate.
[0187] In contrast, if the substrate is only simply cleaned and leveled without being subjected to sufficient roughening treatment (such as the process adopted by the AD-C5 sample), the pull-off strength of the floor coating system is significantly lower, and the failure often occurs at the interface between the coating and the substrate. This indicates that a smooth or insufficiently micro-anchored substrate is difficult to form a strong mechanical bond with the primer coating. Therefore, the substrate pretreatment step emphasized in the present application, which includes a specific surface roughening treatment, is an indispensable key link to ensure that the entire floor system can be firmly attached to the concrete base and exhibit long-term stable use performance. It fundamentally improves the interfacial force between the coating and the substrate and is an important guarantee for improving the durability of the floor.
[0188] Although embodiments of the present application have been shown and described, it is to be understood that various modifications, substitutions, replacements and changes can be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.
Claims
1. A composite material for super wear resistant dust free workshop non-slip floor, characterized in that, The following components in mass fraction: Bio-based resin: 50-70 parts; Self-repairing microcapsule: 5-15 parts; Nano-enhancing and interface modifier: 1-5 parts; Composite wear-resistant aggregate: 20-40 parts; High-hardness polymer: 3-10 parts; Bio-based curing agent: 50-70 parts; Environment-friendly diluent and auxiliary agent: 2-15 parts.
2. A composite material for use in an ultra-wear resistant dust-free workshop anti-skid floor according to claim 1, characterized in that, The bio-based resin is a cardanol-modified vegetable oil-based epoxy resin or a castor oil-based polyurethane prepolymer; the bio-based curing agent is a plant oil fatty acid-modified amine curing agent or a bio-based polyol or polyisocyanate chain extender that chemically reacts with the bio-based resin.
3. A composite material for use in super wear resistant dust free plant floor anti-skid pavement according to claim 1, characterized in that, The wall material of the self-repairing microcapsule is polyurea-formaldehyde or polyurethane, the core material thereof is a mixture containing an epoxy resin repair agent and a latent curing agent, or an isocyanate repair agent, and the average particle size of the self-repairing microcapsule is 20-100 microns.
4. The composite material for super wear resistant dust free plant floor anti-skid pavement according to claim 1, characterized in that, The nano-enhancing and interface modifier is surface-functionalized nano-silica or surface-functionalized nano-carbon tube; the composite wear-resistant aggregate comprises spherical ceramic microbeads and silica-treated corundum particles.
5. The composite material for super wear resistant dust free plant floor anti-skid pavement according to claim 1, characterized in that, The high-hardness polymer is a micrometer-sized particle or short fiber with regular or semi-regular geometry, which is selected from a composite material of polymethyl methacrylate and ceramic powder or a glass fiber reinforced epoxy resin chopped fiber; the environment-friendly diluent and auxiliary agent comprises an active diluent selected from cardanol glycidyl ether or epoxidized soybean oil, a leveling agent selected from a polyether-modified polysiloxane leveling agent, a defoaming agent selected from a mineral oil-based or silicone-based defoaming agent, and a wetting dispersant selected from a high-molecular dispersant with an acidic group.
6. A process for the preparation of a composite material for super wear resistant dust-free workshop anti-skid floor, according to any one of claims 1-5, characterized in that, The following steps are included: S1, base surface pretreatment, including cleaning, leveling, mechanical polishing or shot blasting treatment of the concrete base surface, and ensuring that the base surface is dry; S2, preparation of bio-based penetration-enhancing primer, including mixing the bio-based resin, the bio-based curing agent and the diluent in the environment-friendly diluent and auxiliary agent, and then coating on the pretreated base surface and preliminary curing; S3, preparation of bio-based self-repairing wear-resistant intermediate coating, including uniformly mixing the bio-based resin, self-repairing microcapsule, nano-enhancing and interface modifier, composite wear-resistant aggregate, bio-based curing agent and environment-friendly diluent and auxiliary agent, and then spreading on the primer and curing to form an intermediate coating containing self-repairing microcapsules and composite wear-resistant aggregate; S4, preparation of long-acting anti-slip functional top coating, including uniformly mixing the bio-based resin, nano-enhancing and interface modifier, bio-based curing agent and environment-friendly diluent and auxiliary agent to form a top coating slurry, coating on the intermediate coating, and implanting high-hardness polymer before the top coating slurry is completely cured, and then curing.
7. The process for preparing a composite material for an ultra-wear resistant dust-free workshop anti-skid floor according to claim 6, characterized in that, In the S1 step, the concrete base surface is cleaned to remove oil stains, floating slurry, old coating and loose materials, and leveled; Then, the cleaned and leveled concrete base surface is mechanically polished or shot blasted to form a surface roughness profile of CSP3-5 grade; And before coating the bio-based penetration-enhancing primer, the water content of the base surface is ensured to be less than 5.0%.
8. The process for preparing a composite material for super wear resistant dust free plant floor anti-skid floor according to claim 6, characterized in that, In the S2 step, the bio-based permeation-enhancing primer is applied in an amount of 0.15-0.25 kg / m 2 and its preliminary curing is carried out at ambient temperature of 20-25 °C for 4-8 h until it reaches a tack-free state.
9. The process for preparing a composite material for super wear resistant dust free plant floor anti-skid flooring as claimed in claim 6 wherein, In S3, the paving thickness of the bio-based self-repairing wear-resistant intermediate coating is controlled at 2.0-4.0 mm, and a defoaming roller is used immediately after paving to eliminate bubbles, and then cured at an ambient temperature of 20-25°C for 12-24 h until reaching a recoatable state.
10. The process for preparing a composite material for super wear resistant dust free plant floor anti-skid flooring as claimed in claim 6 wherein, In S4, the bio-based resin, the nano-enhancing and interface modifier, the bio-based curing agent, and the environmentally friendly diluent and auxiliary agent are uniformly mixed to form a top coating slurry, and the top coating slurry is uniformly coated on the intermediate coating by roll coating or blade coating, with the wet film thickness controlled at 0.1-0.3 mm; Before the topcoat slurry reaches a tack-free state, the high-hardness polymer is uniformly implanted into the surface layer of the topcoat slurry by means of precision sowing or electrostatic sanding, with a sowing amount of 100-300 g / m 2 ; Then cured at an ambient temperature of 20-25°C for 24-48 h to form the long-acting anti-skid functional top coating.