A delamination-proof light-weight super-flexible rock plate adhesive and a preparation method thereof
By preparing a lightweight, ultra-flexible slab adhesive, the problem of hollowing and falling off of traditional tile adhesives in the construction of large-size slabs has been solved. It achieves lightweight and high bonding strength, is suitable for the construction of large-size slabs, and meets the requirements of low-carbon green building materials.
Patent Information
- Application Number
- CN202511201573.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-26
- Publication Date
- 2026-02-17
- Estimated Expiration
- 2045-08-26
AI Technical Summary
Traditional tile adhesives are prone to problems such as hollowing and falling off when used in the construction of large-sized slabs. They are also heavy and inconvenient to transport, making it difficult to meet the development needs of low-carbon and green building materials.
The lightweight, ultra-flexible rock slab binder, composed of silicate cement, ceramsite sand, tough resin sand, and dry powder anti-delamination and wetting additives, is prepared through a special process to ensure uniform mixing and bonding strength between the lightweight aggregate and the cementitious material.
It achieves lightweight, anti-delamination, and good crack resistance, with high bonding strength and flexibility, making it suitable for large-size slab construction, reducing hollowing and falling off, and meeting environmental protection requirements.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of binders, in particular to a delamination-preventing light-weight super-flexible rock plate binder and a preparation method thereof. BACKGROUND
[0002] With the improvement of ceramic tile production technology and people's living standards, the hardness requirement of ceramic tiles is getting higher and higher, and the water absorption requirement is getting lower and lower. At the same time, the size of ceramic tiles is gradually increasing. It has become a fashion to replace traditional small tiles with large-size rock plates for indoor decoration, especially high-end decoration. However, rock plate ceramic tiles not only bring visual impact, but also hide physical challenges that ordinary ceramic tile glue cannot cope with. The traditional ceramic tile adhesive on the market has a large dry density (usually greater than 1500 kg / m 3 ), high rigidity, and large shrinkage deformation. When large-size ceramic tiles are laid, the traditional adhesive cannot effectively adapt to the deformation difference caused by the difference in elastic modulus between the base and the ceramic tile due to thermal expansion and cold contraction, which can easily cause the laid ceramic tile to appear hollow, fall off, and other phenomena. In addition, the surface hardness of the traditional ceramic tile adhesive after hardening is high, the strength is large, and the elastic modulus is high, which makes it difficult to resist rapid and large volume shrinkage and even cracking. When large-size ceramic tiles are laid, the adhesive area also increases, which can easily cause the magnification effect to further aggravate the shrinkage and cracking, ultimately leading to ceramic tile bonding failure, which cannot meet the actual engineering needs. During the construction of large-size rock plate ceramic tiles, the amount of adhesive used per unit area is large, which greatly increases the load-bearing capacity of the building. Combined with the continuous gravity traction of heavy rock plate ceramic tiles, the wall load may be seriously overloaded. The traditional ceramic tile adhesive has a safety hazard of hollowing and falling off when laying rock plate type super-large ceramic tiles. At the same time, the large weight of the traditional ceramic tile adhesive product leads to heavy loading and unloading, high transportation costs, and other problems, which do not meet the development direction of low-carbon green building materials.
[0003] Chinese patent CN114477899A discloses "A light ceramic tile glue and its preparation method", the raw material composition includes: coated light sand 140-300 parts by weight, cement 150-280 parts by weight, glue powder 3-25 parts by weight, cellulose ether 2-4 parts by weight, density regulator 10-80 parts by weight; The bulk density of the whole ceramic tile glue is about 900 kg / m³; The above patent solves the problem of uniform mechanical mixing of cement and light aggregate during the mixing and mixing process of ceramic tile glue dry powder, but the cement-based ceramic tile glue needs to be added with water during construction and use, and then a high-speed mixer is used to mix into a pasty viscous slurry (viscosity is usually 300-600 million mPa.S), the light aggregate in the light ceramic tile glue is usually made of light sand, ceramsite sand, expanded perlite, expanded vermiculite, sepiolite, etc., these light aggregates have the characteristics of relatively smooth surface and internal porosity, the smooth surface reduces the area and strength of mechanical occlusion, the internal pores absorb part of the water in the cement slurry, and weaken the interface bonding of cementing material and light aggregate. At the same time, the light aggregate is difficult to disperse uniformly in the viscous paste system, the light aggregate is easy to separate and float up during the high-speed stirring process of adding water, the cement, graded sand, heavy calcium or silica ash is easy to agglomerate and sink after meeting water, so that the cementing material in the ceramic tile glue is difficult to fully and effectively wrap the light aggregate and anchor on the surface of the light aggregate particles, and a high-strength interface transition zone cannot be formed; thereby leading to insufficient strength of the ceramic tile glue, and easy to appear problems such as hollowing and falling off, which has become the main reason for restricting the application of light ceramic tile glue in the market in recent years. SUMMARY
[0004] The main purpose of the present application is to provide a delamination-resistant light super-soft rock plate adhesive and its preparation method, aiming at improving the technical problems such as easy to appear hollowing and falling off when the existing ceramic tile glue is applied to large-size rock plate.
[0005] To achieve the above-mentioned purpose, the present application provides a delamination-resistant light super-soft rock plate adhesive, which comprises the following raw materials in parts by weight: Portland cement 25.0-32.0 parts, sulphoaluminate cement 2.4-3.0 parts, heavy calcium 5.0-8.0 parts, ceramsite sand 35.0-60.0 parts, ductile resin sand 5.0-10.0 parts, dry powder delamination-resistant wetting additive 1.0-2.0 parts, calcium formate 0.5-1.0 parts, suspension stabilizer 0.2-0.5 parts, fumed silica 0.1-0.4 parts, bonding enhancer 0.5-1.0 parts, powder dispersant 0.08-0.2 parts, cellulose ether 0.34-0.4 parts, redispersible latex powder 6.0-10.0 parts, starch ether 0.05-0.1 parts, and wood fiber 0.4-0.8 parts.
[0006] Preferably, the suspension stabilizer is magnesium-aluminum-silicate; the bonding enhancer is silicone powder; and the powder dispersant is sulfonated naphthalene.
[0007] In addition, the application further provides a preparation method of the anti-delamination lightweight super-soft rock plate adhesive, which comprises the following steps: adding silicate cement, heavy calcium, ceramsite sand, tough resin sand, dry powder anti-delamination wetting additive, sulphoaluminate cement, calcium formate, suspension stabilizer, fumed silica, bonding enhancer, powder dispersant, cellulose ether, redispersible latex powder, starch ether and wood fiber into a container according to weight parts, and stirring and uniformly mixing to obtain the anti-delamination lightweight super-soft rock plate adhesive.
[0008] Preferably, the dry powder anti-delamination wetting additive is prepared by the following steps: adding polyethylene glycol 30-40 parts, bamboo charcoal powder 30-45 parts and open-cell expanded perlite 20-30 parts into a container according to weight parts, and fully stirring for 20-25 min; and then adding anti-caking agent 1-5 parts, and stirring for 10-20 min to obtain the dry powder anti-delamination wetting additive.
[0009] Preferably, the bamboo charcoal powder is prepared by high-temperature limited oxygen carbonization treatment as follows: before warming, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min, and flushing for 30 min to displace air, and then vacuuming to 10 Pa; the temperature is raised to 150 ℃ at a temperature raising rate of 4-7 ℃ / min, and dehydrating for 30 min; then the temperature is raised to 280 ℃ at a temperature raising rate of 2-5 ℃ / min, and pre-carbonizing for 40 min; then the temperature is raised to 600 ℃ at a temperature raising rate of 8-12 ℃ / min, and carbonizing for 60 min; and then the temperature is raised to 750 ℃ at a temperature raising rate of 14-17 ℃ / min, and calcining for 2 h to obtain the bamboo charcoal powder.
[0010] Preferably, the anti-caking agent is white carbon black.
[0011] Preferably, the tough resin sand is prepared by the following steps:
[0012] 1) after high-temperature calcination of quartz sand at 850-1000 ℃, 96.2-97.6% of the quartz sand is put into a high-temperature boiling bed, preheated and dehydrated at 200-250 ℃, 0.3-0.5% of silane coupling agent ethanol solution is sprayed, and stirring and grinding is carried out for 20-25 min to obtain pretreated activated aggregate;
[0013] 2) 0.1-0.3% of graphene and 0.5-1.2% of short carbon fiber are added into 1.0-1.2% of bio-based self-hardening furan resin according to weight percentage, ultrasonic oscillation is carried out for 25-30 min, and shearing is carried out for 20-25 min to obtain tough reinforcing resin.
[0014] 3) After the pre-processed activated aggregate is dried, it is put into a sand mixer, and then the toughness-enhancing resin is injected into the sand mixer, and the sand is mixed for 90-100s; then 0.5-0.6% of a lignin sulfonic acid curing agent is added, and the sand is mixed for 45-60s; then magnetic field assisted forming is adopted; then the temperature is controlled to be 70-75℃, and the pre-curing is performed for 12-15min, and then the temperature is cooled to be <50℃ to obtain resin-coated sand;
[0015] 4) After the resin-coated sand is crushed and de-ironed, 70-140 mesh toughness resin sand is obtained.
[0016] Preferably, in step 1), the ethanol accounts for 94.7%, the water accounts for 5%, and the silane accounts for 0.3% in the silane coupling agent ethanol solution by weight percentage.
[0017] Preferably, in step 2), the length of the chopped carbon fiber is 3-5mm.
[0018] Preferably, in step 4), the magnetic field strength during the magnetic field assisted forming is 0.3-0.5T, and the magnetic field strength is maintained for 100-120s.
[0019] Compared with the prior art, the anti-layering lightweight super-flexible rock plate adhesive and the preparation method thereof have the following beneficial effects: the anti-layering lightweight super-flexible rock plate adhesive prepared by the scheme has a lower bulk density and dry density, and the weight is about 1 / 2 of that of a traditional cement-based ceramic tile glue; meanwhile, the dust concentration is low, and the environment is friendly, which not only solves the problem of uneven layering of lightweight ceramic tile glue in the production stirring, packaging and transportation process due to the low self-weight, but also solves the problem of poor lightweight aggregate cohesiveness of lightweight ceramic tile glue in the water stirring and using process, and the uneven wrapping of cementitious materials leads to poor system stability. In addition, the anti-layering lightweight super-flexible rock plate adhesive product has high bonding strength, low elastic modulus, good flexible and anti-cracking performance, better system stability, excellent anti-slippage and longer standing time, can be thin-pasted, and can quickly and efficiently complete the construction of rock plate, and meets the demand of the building industry for high-quality rock plate adhesive products. DETAILED DESCRIPTION
[0020] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0021] In addition, the technical solutions of each embodiment can be combined with each other, but it must be based on the fact that a person skilled in the art can realize it, and when the combination of technical solutions appears to be contradictory or unachievable, it should be considered that the combination of technical solutions does not exist, and is not within the scope of protection required by the present application.
[0022] The anti-delamination light super-soft rock plate adhesive comprises the following raw materials in parts by weight: Portland cement 25.0-32.0 parts, sulphoaluminate cement 2.4-3.0 parts, heavy calcium 5.0-8.0 parts, ceramsite sand 35.0-60.0 parts, tough resin sand 5.0-10.0 parts, dry powder anti-delamination wetting additive 1.0-2.0 parts, calcium formate 0.5-1.0 parts, suspension stabilizer 0.2-0.5 parts, fumed silica 0.1-0.4 parts, bonding enhancer 0.5-1.0 parts, powder dispersant 0.08-0.2 parts, cellulose ether 0.34-0.4 parts, redispersible latex powder 6.0-10.0 parts, starch ether 0.05-0.1 parts and wood fiber 0.4-0.8 parts.
[0023] The anti-delamination light super-soft rock plate adhesive can be applied to various tile sticking fields, and is particularly suitable for laying large-size rock plates.
[0024] The main raw material of the adhesive is Portland cement, and in addition, ceramsite sand is introduced as light aggregate. The ceramsite sand has a special structure of being porous, light in quality, smooth and hard in surface, and has a bulk density of 300-850 kg / m 3 (the bulk density of quartz sand used in a traditional tile adhesive is 1500-2000 kg / m 3 ), and a Mohs hardness of 4-6, which can reduce the bulk density and dry density while ensuring that the adhesive meets the bonding performance and maintains a high strength requirement.
[0025] Sulphoaluminate cement and calcium formate are used in combination as early strength agent to compensate for the delaying effect of polyethylene glycol in the dry powder wetting additive on the early hydration reaction of cement. In a normal temperature environment, the anhydrous calcium sulfate in the sulphoaluminate cement reacts rapidly with gypsum to form ettringite framework, supplemented by CHS gel filling, while the calcium formate can still maintain high activity even in a low temperature environment (≤5℃), and the Ca 2+ / HCOO- ion pair shortens the hydration induction period, accelerates the generation of C-S-H gel, optimizes the pore structure and forms a calcium aluminate enhanced phase, so that the anti-delamination super-soft light rock plate adhesive prepared by the present application still has good early development strength in a winter low temperature construction environment.
[0026] The present application introduces a dry powder anti-delamination wetting additive to prevent the cement and light aggregate from being separated by gravity due to the density difference in the process of packaging, storage and transportation.
[0027] In particular, the present application also introduces a special process to make a tough resin sand as a tough lightweight aggregate, which can effectively make up for the poor toughness caused by the fact that the surface of the ceramic sand in the lightweight super-flexible rock plate adhesive formula is vitreous. As a "soft framework", the long-chain polymer resin of the tough resin sand can absorb energy by stretching, sliding and rearranging when subjected to external force impact, delaying crack propagation. The graphene and short fibers in the resin sand can further enhance the reticular support and bridging effect of the resin sand, effectively preventing the generation of micro-cracks. Combined with lightweight aggregate-ceramic sand, the prepared lightweight super-flexible rock plate adhesive has a bulk density of 760-865 kg / m 3 , which is only 1 / 2 of the bulk density of the traditional cement-based rock plate adhesive, thereby realizing the lightweight of the rock plate adhesive.
[0028] The raw materials of the present application also include fumed silica, which is cross-linked through hydrogen bonds between silicon hydroxyl groups to form a "three-dimensional network framework" throughout the freshly mixed rock plate adhesive slurry. Lightweight aggregate and cement particles are mechanically locked in the network framework, preventing the lightweight aggregate from floating apart when exposed to water and the gravity settling of cement and heavy calcium particles (lying at the bottom). At the same time, the SiO2 on the surface of the fumed silica reacts with the cement hydration product Ca(OH)2 to generate additional calcium silicate hydrate (C-S-H) gel, consuming harmful Ca(OH)2 and preventing the occurrence of efflorescence in the lightweight super-flexible rock plate adhesive.
[0029] The cellulose ether used in the present application can be hydroxyethyl cellulose ether, preferably a product with a viscosity of 12000 mpa.s-30000 mpa.s. The cellulose ether not only brings smooth and lightweight workability to the anti-layering lightweight super-flexible rock plate adhesive, but also promotes the normal progress of the cement hydration reaction of the adhesive under various curing conditions. The excellent water retention performance meets the need for extended air setting time of the anti-layering lightweight super-flexible rock plate adhesive.
[0030] The redispersible latex powder used in the present application can be a high ethylene content vinyl acetate / ethylene copolymer flexible redispersible latex powder, specifically the product with model number 5044N produced by the German Wacker Company. The high ethylene monomer redispersible latex powder can weaken the crystallinity of the polymer chain, form a flexible molecular network, improve the ultimate deformation capacity of the lightweight rock plate adhesive, effectively absorb stress energy to avoid stress concentration, inhibit the propagation of micro-cracks, and give the anti-layering lightweight super-flexible rock plate adhesive of the present application super-strong adhesive force while having good flexibility.
[0031] The starch ether used in the present application is hydroxypropyl starch ether. After water, the hydroxypropyl starch ether rapidly stretches, its hydrophilic groups (-OH / -O-) form a hydrogen bond network with water molecules, the starch ether molecular chain entangles to form a three-dimensional network structure, generates a yield stress, and gives the anti-layering lightweight super-flexible rock plate adhesive good anti-slippage performance.
[0032] The wood fiber used in the present application is a commercially available white fluffy wood fiber (moisture content <5%, heat resistance 230℃) product. When the wood fiber encounters water, the fiber capillary can absorb water and slowly release it to the cement particles, delaying the surface skinning of the slurry, inhibiting the plastic shrinkage of the anti-segregation lightweight super-flexible rock plate adhesive, reducing the cracks caused by the rapid evaporation of early water, and at the same time, the wood fiber is randomly distributed in the mortar to form a micro-tendon network, and the fiber can bridge the cracks to increase the toughness and give the lightweight rock plate adhesive good lateral deformation ability and improve its flexibility.
[0033] In summary, the anti-segregation lightweight super-flexible rock plate adhesive obtained by the above-mentioned formula not only meets the bonding performance, but also has a low bulk density and dry density, and can maintain a high strength requirement. The prepared adhesive has low dust concentration, excellent anti-segregation performance, and the surface of the lightweight aggregate sand and cement powder composition particles forms an agglomerate that does not disperse, avoiding the separation of lightweight super-flexible rock plate adhesive composition due to gravity during production and manufacturing, and even during storage or transportation, the agglomeration and segregation caused by the increase in contact area. While giving the anti-segregation lightweight super-flexible rock plate adhesive good lateral deformation ability, it improves its flexibility performance and meets the standard requirements of flexible adhesive S2. In addition, the anti-segregation lightweight super-flexible rock plate adhesive has low shrinkage, high crack resistance, and can effectively reduce the problems of hollowing, falling, etc. during construction. It can solve the defects of ether wetting additives such as polyethylene glycol that delay the early hydration reaction of cement and slow the development of initial strength. The anti-segregation super-flexible lightweight rock plate adhesive of the present scheme still has good early development strength even in winter low temperature construction environment. The re-dispersible glue powder is enhanced in combination with lightweight aggregate, cement, and heavy calcium filler, has higher bonding strength, meets the C2 type bonding strength requirement, and has no toxic and harmful effects on the environment.
[0034] Further, the suspension stabilizer is magnesium aluminum silicate; the bonding enhancer is silicone powder (specifically, the product with model KJ-B01 produced by Hangzhou Kaijie Plastic Technology Co., Ltd. can be used); and the powder dispersing agent is sulfonated naphthalene.
[0035] The suspension stabilizer used in the embodiment can be specifically magnesium-aluminum silicate suspension stabilizer. When the anti-layering lightweight super-flexible rock plate adhesive is stirred with water, the magnesium-aluminum silicate is dissociated into single-layer or multi-layer nanosheets through silicon-oxygen tetrahedron, aluminum-oxygen tetrahedron and magnesium-oxygen octahedron in the layered structure. The surface of the dissociated silicate sheet layer carries a permanent negative charge, so that a double electric layer (diffusion layer thickness 1-100 nm) is formed around the cement and lightweight aggregate particles in the adhesive, and electrostatic repulsion is generated to resist van der Waals attraction, thereby generating a suspension effect. At the same time, the dissociated nanosheets are randomly stacked in the slurry to form a "card house" structure, which mechanically locks the cement particles in the rock plate adhesive in the grid gap to resist gravity settlement and prevent the cement and lightweight aggregate from layering and settling, thereby ensuring that the cement and other cementitious materials in the rock plate adhesive are fully mixed and uniform.
[0036] The bonding enhancer used in the embodiment can be specifically silicone powder. When the anti-layering lightweight super-flexible rock plate adhesive is stirred with water, the silicone powder releases active silane when it comes into contact with water, which is quickly hydrolyzed into silanol. The silanol can quickly adsorb to the surface of smooth inorganic lightweight aggregate and cement particles. In the alkaline environment system provided by the cement, the silanol forms Si-O-Si bonds through condensation reaction to form a stable inorganic-organic composite structure. After the re-dispersible latex powder is film-formed, the silicone powder and the R group segment are interpenetrated and entangled. The siloxane molecular chain of the silicone powder has flexibility, which can accelerate the fragmentation and crosslinking of the matrix particles into the molecular chain of the re-dispersible latex powder, forming a more compact interface bond to enhance the wrapping bonding force of the re-dispersible latex powder with the lightweight aggregate, cement and heavy calcium filler.
[0037] The powder dispersant used in the embodiment can be specifically sulfonated naphthalene powder dispersant. The dispersant generates compounds with sulfonic acid groups through sulfonation reaction. These molecules are directionally adsorbed to the surface of cement particles, so that the surface of the cement particles carries the same charge, forming an electrostatic repulsion effect to promote the dispersion of cement particles and prevent cement agglomeration and settlement. At the same time, the silicone powder in the anti-layering lightweight super-flexible rock plate adhesive slurry can be fully immersed and adsorbed on the surface of the cement particles, thereby effectively wrapping the above-mentioned lightweight aggregate and re-dispersible latex powder.
[0038] In addition, the application also provides a preparation method of the anti-layering lightweight super-flexible rock plate adhesive, which comprises the following steps: adding silicate cement, heavy calcium, ceramsite sand, ductile resin sand, dry anti-layering wetting additive, sulfur-aluminum cement, calcium formate, suspension stabilizer, fumed silica, bonding enhancer, powder dispersant, cellulose ether, re-dispersible latex powder, starch ether and wood fiber into a container in a weight ratio, and stirring and uniformly mixing to obtain the anti-layering lightweight super-flexible rock plate adhesive. The application has the effect of preventing the lightweight aggregate and cementitious materials from layering during the water stirring process, and ensuring that the lightweight aggregate and cementitious materials in the adhesive are fully mixed and uniform during the water stirring process.
[0039] Specifically, in the production line plowshare type mixing stirrer, using integrated equipment computer calculates the weight and feeding, according to the weight, in turn, 25.0-32.0 parts of Portland cement, 5.0-8.0 parts of heavy calcium, 35-60 parts of ceramsite sand, 5-10 parts of ductile resin sand, 1.0-2.0 parts of dry powder anti-segregation wetting additive, 2.4-3.0 parts of sulphoaluminate cement, 0.5-1 part of calcium formate, 0.2-0.5 part of suspension stabilizer, 0.1-0.4 part of fumed silica, 0.5-1.0 part of bonding enhancer, 0.08-0.2 part of powder dispersant, 0.34-0.4 part of cellulose ether, 6.0-10.0 part of redispersible emulsion powder, 0.05-0.1 part of starch ether, and 0.4-0.8 part of wood fiber are added. According to the above raw material ratio, the stirring bin of the stirrer is put into the stirring bin, the main shaft is stirred at 80 rpm, the high-speed fly cutter is stirred at 1500 rpm, and the mixture is uniformly stirred for 180-240 seconds. After the stirring is completed, the material is discharged and packaged to obtain the anti-segregation lightweight super-flexible rock plate adhesive.
[0040] Further, the dry powder anti-segregation wetting additive is prepared by the following steps: 30-40 parts of polyethylene glycol, 30-40 parts of bamboo charcoal powder, and 20-30 parts of open-cell expanded perlite are added to a container, and stirred for 20-25 minutes; then 1-5 parts of anti-caking agent is added, and stirred for 10-20 minutes to obtain the dry powder anti-segregation wetting additive.
[0041] Specifically, in the preparation of dry powder anti-segregation wetting additive, the stirring speed of the screw belt stirrer pre-dispersion cylinder is adjusted to 400 rpm, 30-40 parts of polyethylene glycol is added first, then 30-45 parts of bamboo charcoal powder and 20-30 parts of open-cell expanded perlite are added in turn, and the powder is fully soaked and uniformly distributed after stirring for 20-25 minutes. The stirring speed of the stirrer is adjusted to 200 rpm to prevent the open-cell expanded perlite from being broken under high-speed stirring; then 1-5 parts of anti-caking agent is slowly added, and stirred for 10-20 minutes to obtain the dry powder anti-segregation wetting additive.
[0042] In the dry powder anti-segregation wetting additive, the environmentally friendly polyethylene glycol PEG400 or PEG600 is used as the wetting component, mainly because polyethylene glycol contains a large number of ether bonds (-O-) and hydroxyl groups (-OH), which can form agglomerates by physical wetting adsorption and hydrogen bonding with cement and lightweight aggregate particles, making the anti-segregation lightweight super-flexible rock plate adhesive more easily stirred uniformly during mechanical mixing, and obtaining a uniformly mixed powder. At the same time, the synergistic effect of polyethylene glycol and water-based additive-redispersible emulsion powder is better, and the biodegradability is better than mineral oil (degradation rate >80%), avoiding the defects such as oily phase separation of silicone oil, industrial white oil and other oily wetting components in the aqueous system.
[0043] In the production process, the polyethylene glycol wetting component-PEG400 / PEG600 is in a viscous liquid state at room temperature, and cannot be directly mixed with cement and lightweight aggregate, the present application transfers PEG400 / PEG600 to porous carrier bamboo charcoal powder and open-cell expanded perlite by carrier transfer method, during the preparation of lightweight super-flexible rock plate adhesive mechanical mixing and stirring, the dry powder of the saturated polyethylene glycol wetting component absorbs the dry powder anti-layering wetting additive, which slowly releases the polyethylene glycol wetting component like a microcapsule, the ether bond oxygen atoms on the long molecular chain of PEG400 / PEG600 are negatively charged, can be adsorbed on the surface of the positively charged cement hydration particles, like countless small anchor points to anchor the lightweight aggregate particles, this adsorption also forms a polymer film on the surface of the powder, prevents the separation of cement and lightweight aggregate, and maintains the flowability of the dry powder to avoid local agglomeration.
[0044] The open-cell expanded perlite with a porous structure and an open honeycomb shape is particularly introduced in the dry powder anti-layering wetting additive, the pores in the open-cell perlite are interconnected, and the oil absorption rate is as high as 200%-500%, which is higher than that of closed-cell expanded perlite, vitrified microbeads and other lightweight materials, and the open-cell expanded perlite is more easily broken by external force, by using this characteristic, the present application is stirred at a speed of 1500 revolutions / minute by a high-speed flying knife of a plow blade type mixing and stirring machine during the preparation of the anti-layering lightweight super-flexible rock plate adhesive, and the open-cell expanded perlite saturated with polyethylene glycol is broken and exploded during the stirring process, and the absorbed polyethylene glycol is fully released into the dry powder of the lightweight rock plate adhesive.
[0045] The present application introduces flexible redispersible emulsion powder of ethylene acetate / ethylene copolymer with high ethylene content, which endows the rock plate adhesive with good transverse deformation ability and improves the flexibility of the rock plate adhesive.
[0046] Further, the bamboo charcoal powder is subjected to high-temperature limited oxygen carbonization treatment as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6L / min for flushing for 30min to replace air, and then vacuumized to 10Pa; the temperature is raised to 150℃ at a temperature raising rate of 4-7℃ / min for dehydration treatment for 30min; then the temperature is raised to 280℃ at a temperature raising rate of 2-5℃ / min for pre-carbonization treatment for 40min; then the temperature is raised to 600℃ at a temperature raising rate of 8-12℃ / min for carbonization treatment for 60min; and then the temperature is raised to 750℃ at a temperature raising rate of 14-17℃ / min for calcination for 2h to obtain the bamboo charcoal powder.
[0047] In this embodiment, the bamboo charcoal powder introduced into the dry powder anti-segregation wetting additive is subjected to high-temperature limited oxygen carbonization treatment through the above steps to make it decompose under anoxic conditions to form a porous structure of carbon material. The treated bamboo charcoal powder molecules have a hexagonal structure, a large specific surface area and surface activity, and strong physical adsorption capacity, with an oil absorption rate of 150%-200% and the ability to effectively saturate and absorb the polyethylene glycol wetting component. In addition, the bamboo charcoal powder particles can act as micro-fine aggregate, effectively filling the gaps between cement particles and ceramsite sand and the tough resin sand, making the mortar structure more compact. The bamboo charcoal powder is soft and can play a role similar to a "bridge" or "obstacle", improving the particle gradation, reducing the original defects and weak points in the binder, and when a micro-crack attempts to expand, it will be forced to change direction or need to bypass the bamboo charcoal powder particles, increasing the resistance to crack propagation and consuming more energy, thereby inhibiting the expansion of the crack, giving the lightweight super-soft rock plate binder good flexibility and ductility, and improving the transverse deformation capacity.
[0048] Further, the anti-caking agent is white carbon black. The present application introduces white carbon black as an anti-caking agent in the dry powder anti-segregation wetting additive, which has a porous structure that can adsorb the bamboo charcoal powder and the excess polyethylene glycol on the surface of the open-cell expanded perlite, reducing the adhesion between particles and maintaining the flowability of the dry powder anti-segregation wetting additive powder. At the same time, the white carbon black particles have a high specific surface area and a high surface charge density, which can significantly increase the friction coefficient between particles and prevent the prepared anti-segregation lightweight super-soft rock plate binder from forming agglomerates and segregation during storage or transportation due to increased contact area.
[0049] Further, the tough resin sand is prepared by the following steps:
[0050] 1) After the quartz sand is calcined at a high temperature of 850-1000°C, 96.2-97.6% of the quartz sand is introduced into a high-temperature fluidized bed, preheated and dehumidified at 200-250°C, and then 0.3-0.5% of a silane coupling agent ethanol solution (0.3%-0.5% of the total weight of the tough resin sand) is sprayed, stirred and ground for 20-25 minutes to obtain a pretreated activated aggregate;
[0051] 2) 0.1-0.3% of graphene and 0.5-1.2% of short carbon fibers are added to 1.0-1.2% of bio-based self-hardening furan resin (specifically, the product with model number XY-SW300 produced by Suzhou Xingye Material Technology Co., Ltd.), and after ultrasonic oscillation for 25-30 minutes, shearing for 20-25 minutes, a tough reinforcing resin is obtained;
[0052] 3) After the pre-processed activated aggregate is dried, it is put into a sand mixer, and the ductile reinforcing resin is injected into the sand mixer, and after mixing for 90-100 seconds, 0.5-0.6% lignin sulfonic acid curing agent is added and mixed for 45-60 seconds, and then magnetic field assisted forming is adopted; the temperature is controlled at 70-75°C, and after pre-curing for 12-15 minutes, the resin coated sand is obtained after cooling to <50°C;
[0053] 4) After the resin coated sand is crushed and de-ironed, the ductile resin sand with a particle size of 70-140 is obtained.
[0054] Specifically, the ductile resin sand is prepared by the following steps: 70-140 mesh quartz sand is calcined at a high temperature of 850-1000°C to remove surface organic impurities and moisture, and then the calcined quartz sand is put into a high-temperature fluidized bed, and after preheating and dehumidifying at 200-250°C, 0.3-0.5% silane coupling agent ethanol solution is sprayed, and the quartz sand is stirred and ground for 20-25 minutes to form an active film on the surface of the quartz sand, and a pre-processed activated aggregate is obtained. 0.1-0.3% graphene and 0.5-1.2% short carbon fiber are added to 1.0-1.2% bio-based self-hardening furan resin in terms of weight percentage, and after ultrasonic oscillation at 40 kHz for 25-30 minutes and starting a high-speed mixer at 8000 revolutions per minute for high-speed shearing for 20-25 minutes, the ductile reinforcing material is uniformly dispersed to avoid agglomeration, and a ductile reinforcing resin is obtained. The pre-processed activated aggregate is heated to 60±5°C in a drying machine, and then put into a continuous sand mixer, and the speed of the continuous sand mixer is adjusted to 300 revolutions per minute, and the ductile reinforcing resin containing graphene and s carbon fiber is injected, and the injection amount is 1.8-2.2%, and the sand is mixed for 90-100 seconds to ensure that the high-speed sanding makes the resin fully wrapped, and the wrapping rate is >95%. Then adjust the speed of the continuous sand mixer to 500 revolutions per minute, slowly add the lignin sulfonic acid curing agent (25-35% of the resin amount), and mix for 45-60 seconds. Then reduce the speed of the continuous sand mixer to 200 revolutions per minute, and since the continuous sand mixer has a permanent magnet / magnetic separation function, the scheme adopts magnetic field assisted forming (start the permanent magnet separator, and set the static magnetic field at 0.3-0.5T through the frequency converter), which induces the carbon fiber to arrange along the principal stress direction, thereby improving the flexibility of the ductile resin sand. After magnetic field assisted forming, the temperature is controlled at 70-75°C, and after pre-curing for 12 minutes, the tensile strength reaches 0.8 MPa, and the resin coated sand is taken out when cooled to <50°C. The resin coated sand prepared is put into a pair roller crusher to crush the solidified material to a particle size of <0.3mm, and a magnetic separator (magnetic field 0.3T) is used to remove iron filings, and then a pneumatic separator is used to extract 70-140 mesh target particles, and finally the ductile resin sand is obtained.
[0055] The toughness resin sand prepared by the process has a bulk density of 600-700 kg / m3 and a Mohs hardness of 4.0, compared with quartz sand used in traditional cement-based rock plate adhesive, the volume density is reduced, and the toughness is 5-10 times higher than that of quartz sand.
[0056] In step 1), the ethanol accounts for 94.7%, the water accounts for 5%, and the silane accounts for 0.3% by weight percentage in the silane coupling agent ethanol solution. In step 2), the length of the chopped carbon fiber is 3 mm. In step 4), the magnetic field strength during the magnetic field assisted forming is 0.3-0.5 T, and the maintaining magnetic field strength is oriented for 100-120 s.
[0057] The technical solutions of the present application are further described in detail in combination with specific embodiments. It should be understood that the following embodiments are only used to explain the present application and do not limit the present application.
[0058] Embodiment 1
[0059] A preparation method of a delamination prevention lightweight super-flexible rock plate adhesive comprises the following steps:
[0060] In the container, 25.0 parts of Portland cement, 8.0 parts of heavy calcium, 48.68 parts of ceramsite sand, 5.0 parts of toughness resin sand, 1.0 part of dry powder delamination prevention wetting additive, 3.0 parts of sulphoaluminate cement, 0.5 part of calcium formate, 0.5 part of suspension stabilizer, 0.4 part of fumed silica, 1.0 part of bonding enhancer, 0.08 part of powder dispersant, 0.34 part of cellulose ether, 6.0 part of redispersible latex powder, 0.1 part of starch ether, and 0.4 part of wood fiber are added, and then they are uniformly stirred and mixed to obtain the delamination prevention lightweight super-flexible rock plate adhesive.
[0061] The dry powder delamination prevention wetting additive is prepared by the following steps: 35 parts of polyethylene glycol, 30 parts of bamboo charcoal powder, and 30 parts of open-cell expanded perlite are added into a container, and then they are fully stirred for 20 min; 5 parts of anti-caking agent is added, and then they are stirred for 10 min to obtain the dry powder delamination prevention wetting additive.
[0062] The bamboo charcoal powder is treated by high-temperature limited oxygen carbonization as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min for flushing for 30 min to displace air, and then vacuum is applied to 10 Pa; the temperature is raised to 150 DEG C at a rate of 5 DEG C / min for dehydration treatment for 30 min; then the temperature is raised to 280 DEG C at a rate of 3 DEG C / min for pre-carbonization treatment for 40 min; then the temperature is raised to 600 DEG C at a rate of 10 DEG C / min for carbonization treatment for 60 min; then the temperature is raised to 750 DEG C at a rate of 15 DEG C / min for calcination for 2 h to obtain the bamboo charcoal powder.
[0063] The tough resin sand is prepared by the following steps: 1) after the quartz sand is calcined at a high temperature of 900 DEG C, 97.6% of the quartz sand is put into a high-temperature boiling bed, preheated and dehumidified at 250 DEG C, and then 0.3% of a silane coupling agent ethanol solution is sprayed, stirred and ground for 25 min to obtain pretreated and activated aggregate; 2) according to the weight percentage, 0.1% of graphene and 0.5% of chopped carbon fiber are added into 1% of bio-based self-hardening furan resin, ultrasonic oscillation is performed for 25 min, and shearing is performed for 20 min to obtain toughness-reinforced resin; 3) after the pretreated and activated aggregate is dried, it is put into a sand mixer, the toughness-reinforced resin is injected into the sand mixer, and sand mixing is performed for 90 s; 0.5% of a lignin sulfonic acid curing agent is added, and sand mixing is performed for 45 s; then, magnetic field assisted forming (the magnetic field strength is 0.5 T, and the magnetic field strength is maintained for 120 s) is adopted; the temperature is controlled to be 75 DEG C, and pre-curing is performed for 12 min, and then cooling is performed to be < 50 DEG C to obtain resin-coated sand; 4) after the resin-coated sand is broken and de-ironed, 70-140 mesh tough resin sand is obtained.
[0064] Example 2
[0065] A preparation method of a delamination-preventing lightweight super-flexible rock plate adhesive comprises the following steps:
[0066] According to the weight parts, silicate cement 27.5 parts, heavy calcium 7.0 parts, ceramsite sand 44.16 parts, tough resin sand 6.5 parts, dry powder delamination-preventing wetting additive 1.3 parts, sulphoaluminate cement 2.8 parts, calcium formate 0.65 parts, suspension stabilizer 0.4 parts, fumed silica 0.3 parts, bonding reinforcing agent 0.8 parts, powder dispersing agent 0.1 parts, cellulose ether 0.36 parts, redispersible latex powder 7.5 parts, starch ether 0.08 parts, and wood fiber 0.55 parts are added into a container, and then they are uniformly stirred and mixed to obtain the delamination-preventing lightweight super-flexible rock plate adhesive.
[0067] The dry powder delamination-preventing wetting additive is prepared by the following steps: according to the weight parts, polyethylene glycol 34 parts, bamboo charcoal powder 35 parts, and open-cell expanded perlite 27 parts are added into a container, and then they are fully stirred for 20 min; then, anti-caking agent 4 parts is added, and then they are stirred for 10 min to obtain the dry powder delamination-preventing wetting additive.
[0068] The bamboo charcoal powder is treated by high-temperature limited oxygen carbonization as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min for flushing for 30 min to displace air, and then vacuum is extracted to 10 Pa; the temperature is raised to 150 DEG C at a rate of 5 DEG C / min for dehydration treatment for 30 min; then, the temperature is raised to 280 DEG C at a rate of 3 DEG C / min for pre-carbonization treatment for 40 min; then, the temperature is raised to 600 DEG C at a rate of 10 DEG C / min for carbonization treatment for 60 min; then, the temperature is raised to 750 DEG C at a rate of 15 DEG C / min for calcination for 2 h to obtain the bamboo charcoal powder.
[0069] The tough resin sand is prepared by the following steps: 1) after the quartz sand is calcined at a high temperature of 900°C, the 97.6% of the quartz sand is put into a high-temperature boiling bed, preheated and dehumidified at 250°C, sprayed with 0.3% of a silane coupling agent ethanol solution, stirred and ground for 25 min to obtain pretreated activated aggregate; 2) according to the weight percentage, 0.1% of graphene and 0.5% of short carbon fiber are added into 1% of bio-based self-hardening furan resin, ultrasonic oscillation is performed for 25 min, and shearing is performed for 20 min to obtain tough reinforced resin; 3) after the pretreated activated aggregate is dried and put into a sand mixer, the tough reinforced resin is injected into the sand mixer, sand mixing is performed for 90 s, 0.5% of a lignin sulfonic acid curing agent is added, sand mixing is performed for 45 s, then magnetic field assisted forming (magnetic field strength is 0.5T, maintaining the magnetic field strength direction for 120 s) is adopted, the temperature is controlled to be 75°C, and pre-curing is performed for 12 min, and then cooling to <50°C to obtain resin-coated sand; 4) after the resin-coated sand is broken and de-ironed, 70-140 mesh tough resin sand is obtained.
[0070] Example 3
[0071] A preparation method of a delamination-resistant light-weight super-flexible rock plate adhesive comprises the following steps:
[0072] According to the weight parts, 30 parts of Portland cement, 6.0 parts of heavy calcium, 40.61 parts of ceramsite sand, 8.0 parts of tough resin sand, 1.6 parts of dry powder delamination-resistant wetting additive, 2.6 parts of sulphoaluminate cement, 0.8 parts of calcium formate, 0.3 parts of suspension stabilizer, 0.2 parts of fumed silica, 0.65 parts of bonding enhancer, 0.15 parts of powder dispersant, 0.38 parts of cellulose ether, 8.0 parts of redispersible latex powder, 0.06 parts of starch ether, and 0.65 parts of wood fiber are added into a container, and then uniformly stirred and mixed to obtain a delamination-resistant light-weight super-flexible rock plate adhesive.
[0073] The dry powder delamination-resistant wetting additive is prepared by the following steps: according to the weight parts, 32 parts of polyethylene glycol, 40 parts of bamboo charcoal powder, and 25 parts of open-cell expanded perlite are added into a container, and then fully stirred for 25 min; 3 parts of an anti-caking agent are further added, and then stirred for 15 min to obtain the dry powder delamination-resistant wetting additive.
[0074] The bamboo charcoal powder is treated by high-temperature oxygen-limited carbonization as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min for 30 min to displace air, and then vacuum is applied to 10 Pa; the temperature is raised to 150 ℃ at a rate of 5 ℃ / min, and constant temperature is maintained for 30 min for dehydration treatment; then the temperature is raised to 280 ℃ at a rate of 3 ℃ / min, and constant temperature is maintained for 40 min for pre-carbonization treatment; then the temperature is raised to 600 ℃ at a rate of 10 ℃ / min, and constant temperature is maintained for 60 min for carbonization treatment; then the temperature is raised to 750 ℃ at a rate of 15 ℃ / min, and constant temperature is maintained for 2 h for calcination to obtain the bamboo charcoal powder.
[0075] The ductile resin sand is prepared by the following steps: 1) after the quartz sand is calcined at a high temperature of 900 ℃, the 97.6% of the quartz sand is put into a high-temperature boiling bed, preheated and dehumidified at 250 ℃, sprayed with 0.3% of a silane coupling agent ethanol solution, stirred and ground for 25 min to obtain pretreated activated aggregate; 2) according to the weight percentage, 0.1% of graphene and 0.5% of short carbon fibers are added into 1.0% of bio-based self-hardening furan resin, ultrasonic oscillation is performed for 25 min, and shearing is performed for 20 min to obtain ductile reinforced resin; 3) after the pretreated activated aggregate is dried and put into a sand mixer, the ductile reinforced resin is injected into the sand mixer, sand mixing is performed for 90 s, 0.5% of a lignin sulfonic acid curing agent is added, sand mixing is performed for 45 s, then magnetic field assisted forming is adopted (the magnetic field strength is 0.5 T, and the magnetic field strength is maintained for 120 s), the temperature is controlled to be 75 ℃, and pre-curing is performed for 12 min, and then cooling is performed to be < 50 ℃ to obtain resin-coated sand; 4) after the resin-coated sand is broken and de-ironed, 70-140 mesh ductile resin sand is obtained.
[0076] Example 4
[0077] A preparation method of a delamination-preventing lightweight super-soft rock plate adhesive includes the following steps:
[0078] According to weight parts, silicate cement 32 parts, heavy calcium 5.0 parts, ceramsite sand 35.35 parts, ductile resin sand 10.0 parts, dry powder delamination-preventing wetting additive 2.0 parts, sulphoaluminate cement 2.4 parts, calcium formate 1.0 part, suspension stabilizer 0.2 part, fumed silica 0.1 part, bonding enhancer 0.5 part, powder dispersant 0.2 part, cellulose ether 0.4 part, redispersible latex powder 10.0 part, starch ether 0.05 part, and wood fiber 0.80 part are added into a container, and then stirred and mixed uniformly to obtain the delamination-preventing lightweight super-soft rock plate adhesive.
[0079] The dry powder delamination-preventing wetting additive is prepared by the following steps: according to weight parts, polyethylene glycol 33 parts, bamboo charcoal powder 45 parts, and open-cell expanded perlite 20 parts are added into a container, and then stirred for 25 min; then anti-caking agent 2 parts is added, and stirred for 20 min to obtain the dry powder delamination-preventing wetting additive.
[0080] The bamboo charcoal powder is treated by high-temperature oxygen-limited carbonization as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min for flushing for 30 min to displace air, and then vacuum is drawn to 10 Pa; the temperature is raised to 150 ℃ at a rate of 5 ℃ / min, and constant temperature is maintained for 30 min for dehydration treatment; then the temperature is raised to 280 ℃ at a rate of 3 ℃ / min, and constant temperature is maintained for 40 min for pre-carbonization treatment; then the temperature is raised to 600 ℃ at a rate of 10 ℃ / min, and constant temperature is maintained for 60 min for carbonization treatment; then the temperature is raised to 750 ℃ at a rate of 15 ℃ / min, and constant temperature is maintained for 2 h for calcination to obtain the bamboo charcoal powder.
[0081] The tough resin sand is prepared by the following steps: 1) after the quartz sand is calcined at a high temperature of 900 ℃, the 97.6% of the quartz sand is put into a high-temperature fluidized bed, preheated and dehumidified at 250 ℃, sprayed with 0.3% of a silane coupling agent ethanol solution, and stirred and ground for 25 min to obtain pretreated activated aggregate; 2) according to the weight percentage, 0.1% of graphene and 0.5% of chopped carbon fiber are added into 1.0% of bio-based self-hardening furan resin, ultrasonic oscillation is performed for 25 min, and shearing is performed for 20 min to obtain tough reinforcing resin; 3) the pretreated activated aggregate is dried and put into a sand mixer, the tough reinforcing resin is injected into the sand mixer, and sand mixing is performed for 90 s; 0.5% of a lignin sulfonic acid curing agent is added, sand mixing is performed for 45 s, magnetic field assisted forming is adopted (magnetic field strength is 0.5 T, and the magnetic field strength is maintained for 120 s), the temperature is controlled to be 75 ℃, and pre-curing is performed for 12 min, and then cooling is performed to be < 50 ℃ to obtain resin-coated sand; 4) after the resin-coated sand is broken and de-ironed, 70-140 mesh tough resin sand is obtained.
[0082] The anti-layering light weight super-flexible rock plate adhesive prepared in examples 1-4 is subjected to the following performance detection, and the specific detection results are shown in the following table:
[0083]
[0084] Note: 1. The bulk density and dry density of the adhesive are evaluated according to the provisions of JG / T521-2017 “Lightweight Mortar” type C.
[0085] 2. The flexibility, slip, extended curing time performance, and bonding strength of the adhesive are evaluated according to the standard of JC / T547-2017 “Ceramic Tile Adhesive” C2TES1 flexible anti-slip extended curing time enhanced cement-based adhesive.
[0086] 3. The formaldehyde release amount and total volatile organic compound (TVOC) release amount of the adhesive are evaluated according to the technical index requirements of T / CCIA0028-2025 “Rock Plate Adhesive”.
[0087] 4. The shrinkage of the adhesive is evaluated according to the standard requirements of T / SZWA001-2017 "Polymer Mortar".
[0088] 5. The bagging dust concentration of the adhesive is determined according to the method in JJG846-2015 "Dust Concentration Measuring Instrument Verification Regulation".
[0089] According to the test results of each example in the above table, the bulk density and dry density of the anti-delamination lightweight super-flexible rock plate adhesive prepared in Examples 1-4 are smaller, which has the characteristics of lightweight; in addition, the slip is less, the transverse deformation ability S2 is above 5.5, the bonding strength is higher, the formaldehyde release amount is lower, the total volatile organic compounds are less, the shrinkage is lower, and the bagging dust concentration is relatively smaller.
[0090] Comparative Example 1
[0091] The traditional adhesive includes the following raw materials in parts by weight: Portland cement 32 parts, heavy calcium 10 parts, 70-140 mesh quartz sand 48.67 parts, calcium formate 0.5 parts, cellulose ether 0.35 parts, redispersible latex powder 8.0 parts, starch ether 0.08 parts, and wood fiber 0.4 parts.
[0092] Comparative Example 2
[0093] In this comparative example, the preparation steps and parameters are the same as those of Example 1, except that 70-140 mesh quartz sand 53.68 parts is used instead of the ceramic sand and the tough resin sand of Example 1.
[0094] Comparative Example 3
[0095] In this comparative example, the preparation steps and parameters are the same as those of Example 2, except that heavy calcium powder is used instead of the dry powder anti-delamination wetting additive, i.e., the heavy calcium powder is increased to 8.3 parts.
[0096] Comparative Example 4
[0097] In this comparative example, the preparation steps and parameters are the same as those of Example 3, except that ceramic sand is used instead of the tough resin sand, i.e., the ceramic sand is increased to 48.61 parts.
[0098] Comparative Example 5
[0099] In this comparative example, the preparation steps and parameters are the same as those of Example 4, except that heavy calcium powder is used instead of the bonding enhancer and the powder dispersant, i.e., the ceramic sand is increased to 48.61 parts.
[0100] Comparative Example 6
[0101] The preparation steps and parameters in the present comparative example are the same as those in Example 1, except that the untreated conventional bamboo charcoal powder is directly used in Comparative Example 6, i.e., the high-temperature limited-oxygen carbonization treatment process of the bamboo charcoal powder is cancelled.
[0102] Comparative Example 7
[0103] The preparation steps and parameters in the present comparative example are the same as those in Example 1, except that the magnetic field assisted forming process is not performed in Comparative Example 7.
[0104] The adhesive prepared in Comparative Examples 1-7 is subjected to the following performance tests, and the specific test results are shown in the following table:
[0105]
[0106] According to the test results of the comparative examples in the above table, the bulk density and dry density of Examples 1-4 are smaller than those of the traditional ceramic tile adhesive in Comparative Example 1, the adhesive strength is maintained in a good range while maintaining lightweight, the shrinkage rate is maintained below 0.15%, and the bag dust concentration is maintained below 60 mg / m3, which are all better than those of the traditional ceramic tile adhesive in Comparative Example 1.
[0107] Example 1 uses the formulation of lightweight aggregate ceramsite sand and ductile resin sand compared with Comparative Example 2, the bulk density and dry density meet the standard requirements of lightweight mortar, the bulk density is about 1 / 2 of the ceramic tile glue in Comparative Example 2, and the weight is reduced by half of the ceramic tile glue in Comparative Example 2. The formulation of quartz sand used in Comparative Example 2 has poor flexibility and does not meet the standard requirements of flexible adhesive S2.
[0108] Example 2 adds a dry powder anti-segregation wetting additive formulation with a low bag dust concentration, cement and lightweight aggregate ceramsite sand, and ductile resin sand are uniformly adsorbed and wrapped, and the adhesive strength is high; at the same time, the shrinkage rate is low, which meets the standard requirements. Comparative Example 3 does not add a dry powder anti-segregation wetting agent, the bag dust concentration is more than 20 times that of Example 2, the dust segregation is obvious, and the shrinkage rate does not meet the standard requirements, the adhesive strength is about 35% lower than that of Example 2, and the cement and lightweight aggregate are separated and uneven.
[0109] Example 3 uses ductile resin sand compared with Comparative Example 4, the overall formulation has good flexibility and meets the standard requirements of flexible adhesive S2; Comparative Example 4 does not add ductile resin sand, the flexibility is relatively poor and does not meet the S2 standard requirements, and the shrinkage rate is higher than that of Example 3.
[0110] Example 4 adds a bonding enhancer and a powder dispersant compared with Comparative Example 5, and the overall adhesive strength is high; Comparative Example 5 does not add a bonding enhancer and a powder dispersant, and the adhesive strength is about 33.3% lower than that of Example 4.
[0111] Compared with Comparative Example 6, the transverse deformation ability S2 of the ceramic tile adhesive is reduced and the bag dust concentration is increased when the conventional bamboo charcoal powder is used.
[0112] Compared with Comparative Example 7, the transverse deformation ability S2 of the ceramic tile adhesive is reduced when the magnetic field assisted forming is not performed.
[0113] Example 5
[0114] In this embodiment, the preparation steps and parameters are the same as those in Example 1, except that the high-temperature limited-oxygen carbonization heating rate of the bamboo charcoal powder in Example 5 is adjusted, and the specific adjustment is as follows:
[0115]
[0116] The anti-layering lightweight super-flexible rock plate adhesive prepared in Example 5 is subjected to performance detection, and the specific detection results are shown in the following table:
[0117]
[0118] As shown in the test data in the above table, adjusting the high-temperature limited-oxygen carbonization treatment parameters of the bamboo charcoal powder will have a certain influence on the bag dust concentration of the anti-layering lightweight super-flexible rock plate adhesive. The preferred high-temperature limited-oxygen carbonization treatment parameters of the bamboo charcoal powder in this scheme are as follows: dehydrating at a constant temperature of 150°C for 30 min with a heating rate of 6°C / min; pre-carbonizing at a constant temperature of 280°C for 40 min with a heating rate of 4°C / min; carbonizing at a constant temperature of 600°C for 60 min with a heating rate of 12°C / min; and calcining at a constant temperature of 750°C for 2 h with a heating rate of 16°C / min to obtain the bamboo charcoal powder. The bamboo charcoal powder obtained under the above preparation parameters has a strong physical adsorption capacity, which can improve the flexibility of the anti-layering lightweight super-flexible rock plate adhesive, reduce the bag dust concentration, and mix the cement and lightweight aggregate more uniformly.
[0119] Example 6
[0120] A preparation method of an anti-layering lightweight super-flexible rock plate adhesive, comprising the following steps:
[0121] In a container, 28 parts of Portland cement, 5 parts of heavy calcium, 39.57 parts of ceramsite sand, 10 parts of ductile resin sand, 2 parts of anti-layering wetting additive, 2.4 parts of sulphoaluminate cement, 0.5 parts of calcium formate, 0.3 parts of suspension stabilizer, 0.2 parts of fumed silica, 1 part of bonding enhancer, 0.1 part of powder dispersant, 0.37 parts of cellulose ether, 10 parts of redispersible emulsion powder, 0.06 parts of starch ether, and 0.5 parts of wood fiber are added by weight, and then uniformly mixed to obtain an anti-layering lightweight super-flexible rock plate adhesive.
[0122] The dry powder anti-segregation wetting additive is prepared by the following steps: adding 40 parts of polyethylene glycol, 38 parts of bamboo charcoal powder and 20 parts of open-cell expanded perlite into a container by weight parts, and stirring thoroughly for 25 min; then adding 2 parts of an anti-caking agent, and stirring for 20 min to obtain the dry powder anti-segregation wetting additive.
[0123] The bamboo charcoal powder is treated by high-temperature limited oxygen carbonization as follows: before warming up, nitrogen gas is introduced into the furnace at a flow rate of 6 L / min for flushing for 30 min to displace air, and then vacuumized to 10 Pa; the temperature is raised to 150°C at a rate of 6°C / min for dehydration treatment; then the temperature is raised to 280°C at a rate of 4°C / min for pre-carbonization treatment for 40 min; then the temperature is raised to 600°C at a rate of 12°C / min for carbonization treatment for 60 min; and then the temperature is raised to 750°C at a rate of 16°C / min for calcination for 2 h to obtain the bamboo charcoal powder.
[0124] The ductile resin sand is prepared by the following steps: 1) after the quartz sand is baked at a high temperature of 900°C, the 96.4% quartz sand is put into a high-temperature boiling bed, preheated and dehumidified at 250°C, sprayed with 0.3% silane coupling agent ethanol solution, and stirred and ground for 25 min to obtain pretreated activated aggregate; 2) 0.3% graphene and 1.2% short carbon fiber are added into 1.2% bio-based self-hardening furan resin by weight percentage, and after ultrasonic oscillation for 25 min, shearing for 20 min, a ductile reinforced resin is obtained; 3) the pretreated activated aggregate is dried and put into a sand mixer, and the ductile reinforced resin is injected into the sand mixer, and after mixing for 90 s, 0.6% lignin sulfonic acid curing agent is added and mixed for 45 s; then magnetic field assisted forming is adopted (magnetic field strength is 0.5 T, and the magnetic field strength is maintained for 120 s); then the temperature is controlled at 75°C, and pre-curing is performed for 12 min, and then cooling to <50°C to obtain resin-coated sand; 4) after crushing and removing iron, the resin-coated sand is obtained as 70-140 mesh ductile resin sand.
[0125] The anti-segregation light super-soft rock plate adhesive prepared in Example 6 is subjected to performance detection, and the specific detection results are shown in the following table:
[0126]
[0127] From the test results of the above table, by comprehensively optimizing the raw materials, the ratio, the preparation parameters of the dry powder anti-layering wetting additive, the high temperature oxygen limiting carbonization process of the bamboo charcoal powder and the preparation parameters of the tough resin sand of the anti-layering light super flexible rock plate adhesive, the bulk density and dry density of the prepared anti-layering light super flexible rock plate adhesive can be maintained within the appropriate range, the flexibility of the adhesive S2 is maintained at 6.5mm, the bonding strength is higher, and the formaldehyde release and the content of total volatile organic compounds are lower.
[0128] The above only describes the preferred embodiments of the present application, and does not limit the patent scope of the present application. Any equivalent structural transformation, direct / indirect application in other related technical fields, or direct / indirect application in other related technical fields based on the inventive concept of the present application are included in the patent protection scope of the present application.
Claims
1. A delamination resistant lightweight superflexible rock board adhesive, characterized by, By weight parts, including the following raw materials: Portland cement 25.0-32.0 parts, sulphoaluminate cement 2.4-3.0 parts, heavy calcium 5.0-8.0 parts, ceramsite sand 35.0-60.0 parts, ductile resin sand 5.0-10.0 parts, dry powder anti-segregation wetting additive 1.0-2.0 parts, calcium formate 0.5-1.0 parts, suspension stabilizer 0.2-0.5 parts, fumed silica 0.1-0.4 parts, bonding enhancer 0.5-1.0 parts, powder dispersant 0.08-0.2 parts, cellulose ether 0.34-0.4 parts, redispersible latex powder 6.0-10.0 parts, starch ether 0.05-0.1 parts, wood fiber 0.4-0.8 parts; the bonding enhancer is silicone powder; The ductile resin sand is prepared by the following steps: 1) after the quartz sand is calcined at a high temperature of 850-1000℃, 96.2%-97.6% of the quartz sand is put into a high-temperature boiling bed, preheated and dehumidified at 200-250℃, sprayed with 0.3-0.5% of a silane coupling agent ethanol solution, stirred and ground for 20-25min to obtain pretreated activated aggregate; 2) according to the weight percentage, 0.1-0.3% of graphene and 0.5-1.2% of short carbon fiber are added into 1-1.2% of bio-based self-hardening furan resin, ultrasonic oscillation is performed for 25-30min, and shearing is performed for 20-25min to obtain a ductile reinforcing resin; 3) the pretreated activated aggregate is dried and put into a sand mixer, the ductile reinforcing resin is injected into the sand mixer, sand mixing is performed for 90-100s, 0.5-0.6% of a lignin sulfonic acid curing agent is added, and sand mixing is performed for 45-60s; then magnetic field assisted forming is adopted; the temperature is controlled at 70-75℃, pre-curing is performed for 12-15min, and cooling is performed to <50℃ to obtain resin-coated sand; 4) after the resin-coated sand is crushed and de-ironed, the 70-140 mesh ductile resin sand is obtained; The dry powder anti-segregation wetting additive is prepared by the following steps: according to weight parts, polyethylene glycol 30-40 parts, bamboo charcoal powder 30-45 parts, and open-cell expanded perlite 20-30 parts are added into a container, and fully stirred for 20-25min; then anti-caking agent 1-5 parts is added, stirred for 10-20min to obtain the dry powder anti-segregation wetting additive; The bamboo charcoal powder is treated by high-temperature limited oxygen carbonization as follows: nitrogen gas is introduced into the furnace to replace air, and then vacuum is applied; the temperature is raised to 150℃ at a rate of 4-7℃ / min, and constant temperature is maintained for 30min for dehydration treatment; then the temperature is raised to 280℃ at a rate of 2-5℃ / min, and constant temperature is maintained for 40min for pre-carbonization treatment; then the temperature is raised to 600℃ at a rate of 8-12℃ / min, and constant temperature is maintained for 60min for carbonization treatment; then the temperature is raised to 750℃ at a rate of 14-17℃ / min, and constant temperature is maintained for 2h for calcination to obtain the bamboo charcoal powder.
2. A delamination resistant lightweight superflexible rock board adhesive according to claim 1, characterized in that, The suspension stabilizer is magnesium aluminum silicate; the powder dispersant is sulfonated naphthalene.
3. A delamination resistant lightweight superflexible rock board adhesive according to claim 1, wherein The anti-caking agent is white carbon black.
4. The anti delamination lightweight super flexible rock board adhesive according to claim 1, wherein, In step 1), the ethanol accounts for 94.7%, the water accounts for 5%, and the silane accounts for 0.3% in the silane coupling agent ethanol solution by weight percentage.
5. The anti delamination lightweight super flexible rock board adhesive as claimed in claim 1, wherein, In step 2), the length of the short carbon fiber is 3-5mm.
6. The anti delamination lightweight super flexible rock board adhesive as claimed in claim 1, wherein, In step 4), the magnetic field strength during the magnetic field assisted forming is 0.3-0.5T, and the maintaining magnetic field strength is oriented for 100-120s.
7. A process for the preparation of a delamination resistant lightweight superflexible rock board adhesive as claimed in any one of claims 1 to 2, characterized in that, The method comprises the following steps: adding silicate cement, heavy calcium, ceramsite sand, tough resin sand, dry powder anti-segregation wetting additive, sulphoaluminate cement, calcium formate, suspension stabilizer, fumed silica, bonding enhancer, powder dispersant, cellulose ether, redispersible emulsion powder, starch ether and wood fiber into a container in parts by weight, and uniformly mixing to obtain the anti-segregation lightweight super-flexible rock plate bonding agent.
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