Raw material of soft porcelain material prepared from hemp stalks, soft porcelain material prepared from hemp stalks and preparation method of soft porcelain material
By using alkali-modified hemp stalk powder and other raw materials to prepare soft ceramic materials, a three-dimensional network structure is formed, which solves the shortcomings of existing soft ceramic materials in terms of flexibility, wear resistance and water impermeability, and achieves an improvement in overall performance.
Patent Information
- Application Number
- CN202510902364.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-01
- Publication Date
- 2025-11-11
AI Technical Summary
Existing soft ceramic materials cannot simultaneously meet the requirements for use in terms of flexibility, wear resistance, flame retardancy and water impermeability, and have a high water absorption rate, which affects durability.
Using alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, curing agent, dispersant, film-forming aid, and waterproofing agent as main raw materials, a three-dimensional network structure is formed through cross-linking reaction to prepare a soft ceramic material with good comprehensive performance.
It improves the flexibility, wear resistance, flame retardancy, and water impermeability of flexible ceramic materials, enhancing the overall performance of the materials and meeting the requirements for the use of low-carbon decorative materials.
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Figure BDA0005477529990000141
Abstract
Description
Technical Field
[0001] This invention relates to the field of building materials technology, and in particular to a raw material for a soft porcelain material made from hemp stalks, the soft porcelain material made from hemp stalks, and a method for preparing the same. Background Technology
[0002] Flexible ceramic tile is a new type of environmentally friendly building decoration material. This material combines the advantages of traditional ceramic tiles and flexible decorative materials, featuring lightweight, flexibility, strong weather resistance, and ease of installation, making it suitable for both indoor and outdoor wall decoration. Compared to traditional ceramic tiles and most decorative materials that are difficult to degrade, this material, after a certain number of years of use, or when its style or color needs to be updated, can be completely recycled and reprocessed into new products or restored to ordinary sand, meeting the requirements of returning to nature. It is a low-carbon and environmentally friendly decorative material with broad promotional value.
[0003] Currently available flexible ceramic materials have poor moisture regulation capabilities and high water absorption rates, making it difficult to meet the waterproof requirements of the flexible ceramic industry standard. Moreover, prolonged exposure to moisture will reduce the durability of flexible ceramic materials, thereby shortening their service life. In addition, the flexibility, wear resistance, and flame retardant properties of existing flexible ceramic materials are also difficult to meet customer requirements.
[0004] Therefore, developing a low-carbon decorative material that combines flexibility, wear resistance, flame retardancy, and water impermeability is of great significance to the field of building decoration materials. Summary of the Invention
[0005] The main objective of this invention is to propose a raw material for a flexible ceramic material made from hemp stalks, the flexible ceramic material made from hemp stalks, and a method for preparing the same material, aiming to solve the problem that existing low-carbon decorative materials cannot simultaneously meet the requirements for flexibility, wear resistance, flame retardancy, and water impermeability.
[0006] To achieve the above objectives, this invention proposes a soft ceramic material made from hemp stalks. The raw materials for the soft ceramic material made from hemp stalks include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, curing agent, dispersant, film-forming aid, and waterproofing agent; wherein the mineral powder includes granite powder, quartz powder, and corundum powder.
[0007] In one embodiment, the raw materials for the soft ceramic material made from hemp stalks include the following components in parts by weight:
[0008] The composition includes: 70-150 parts alkali-modified hemp stalk powder, 180-220 parts granite powder, 500 parts quartz powder, 100 parts corundum powder, 50 parts inorganic filler, 30 parts organophosphorus flame retardant, 0.3-9 parts coupling agent, 2-10 parts first emulsion, 10-15 parts second emulsion, 0.1-0.4 parts curing agent, 0.1-0.4 parts dispersant, 0.1-0.4 parts film-forming aid, and 0.1-0.4 parts waterproofing agent.
[0009] In one embodiment, the alkali-modified hemp stalk powder is prepared according to the following steps:
[0010] Dry hemp stalks are soaked in an alkaline solution to obtain alkaline-treated hemp stalks. The alkaline-treated hemp stalks are then dried and pulverized to obtain alkali-modified hemp stalk powder.
[0011] In one embodiment, the alkaline solution is a 10%–15% aqueous sodium hydroxide solution, and the mass ratio of the dried hemp stalks to the alkaline solution is 1:(5–10); and / or,
[0012] The soaking time is 0.3–1 hour; and / or,
[0013] The soaking temperature is 50–80°C.
[0014] In one embodiment, the particle size of the alkali-modified hemp stalk powder is 300 mesh to 400 mesh; and / or,
[0015] The quartz powder has a fineness of 200 mesh to 6000 mesh; and / or,
[0016] The granite powder has a fineness of 60 mesh to 100 mesh; and / or,
[0017] The fineness of the corundum powder is 60 mesh to 120 mesh.
[0018] In one embodiment, the inorganic filler comprises at least one of modified aluminum hydroxide and modified magnesium hydroxide; and / or,
[0019] The first emulsion comprises a polyurethane emulsion, and the second emulsion comprises at least one selected from vinyl acetate-acrylic emulsion, pure acrylic emulsion, ethylene-vinyl acetate copolymer emulsion, styrene-acrylic emulsion, and vinyl acetate emulsion; and / or,
[0020] The organophosphorus flame retardant includes phosphate ester flame retardants; and / or,
[0021] The coupling agent includes at least two of titanate coupling agents, aluminate coupling agents, and silane coupling agents; and / or,
[0022] The curing agent includes any one of aziridine curing agents, polycarbodiimide curing agents, and isocyanate curing agents; and / or,
[0023] The dispersant includes sodium polycarboxylate type dispersants; and / or,
[0024] The film-forming aid includes at least one selected from 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, benzyl alcohol, and dibutyl phthalate; and / or...
[0025] The waterproofing agent includes silicone-based waterproofing agents.
[0026] This invention proposes a method for preparing a soft ceramic material using hemp stalks, employing the raw materials described in the aforementioned technical solution. The method for preparing the soft ceramic material using hemp stalks includes the following steps:
[0027] The coupling agent is dispersed in an alcohol solution to obtain a coupling agent solution; alkali-modified hemp stalk powder, mineral powder and inorganic filler are mixed to obtain a mixed powder; the coupling agent solution is added to the mixed powder to obtain a first mixture;
[0028] A curing agent, dispersant, film-forming aid, and water are mixed to obtain a second mixture. Then, an organophosphorus flame retardant, a first emulsion, a second emulsion, and a waterproofing agent are added to the second mixture to obtain a third mixture.
[0029] The first mixture and the third mixture are mixed to obtain a slurry;
[0030] The slurry is poured into a mold, pressed into shape, dried, and demolded to obtain the soft ceramic material made from hemp stalks.
[0031] In one embodiment, the compression molding pressure is 3–15 MPa; and / or,
[0032] The pressing temperature is 50–70°C; and / or,
[0033] The pressing and molding time is 0.3 to 0.5 hours.
[0034] In one embodiment, the drying temperature is 40–80°C; and / or,
[0035] The drying time is 4 to 16 hours.
[0036] This invention proposes a soft ceramic material made from hemp stalks, which is prepared according to the preparation method of soft ceramic material made from hemp stalks described in the foregoing technical solution.
[0037] In the technical solution of this invention, the raw materials for the soft ceramic material made from hemp stalks include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, and additives. The mineral powder includes granite powder, quartz powder, and corundum powder. Alkali-modified hemp stalk powder, mineral powder, inorganic filler, and organophosphorus flame retardant are the main raw materials, while curing agent, dispersant, film-forming aid, and waterproofing agent are used as additives. The coupling agent is used to organically process the surfaces of the alkali-modified hemp stalk powder, mineral powder, and inorganic filler, improving their compatibility with other organic materials. These powders modified by the coupling agent then undergo a cross-linking reaction under the combined action of the organophosphorus flame retardant, first emulsion, second emulsion, and additives to form a three-dimensional network structure, thus obtaining the soft ceramic material made from hemp stalks. This invention improves the flexibility, abrasion resistance, cigarette burn resistance, scratch resistance, and water impermeability of flexible ceramic materials by modifying hemp stalk powder with alkali. Mineral powder serves as the main structural base of the flexible ceramic material, providing hardness, strength, and abrasion resistance. Granite powder enhances the abrasion resistance, cigarette burn resistance, scratch resistance, and water impermeability of the flexible ceramic material. Organophosphorus flame retardants improve flame retardancy while simultaneously enhancing the abrasion resistance, cigarette burn resistance, and water impermeability of the flexible ceramic material. Inorganic fillers improve the fire resistance, mechanical properties, and thermal stability of the material. Compared with conventional flexible ceramic materials, the raw materials used in this invention, which utilize hemp stalks, facilitate the production of flexible ceramic materials with excellent comprehensive performance, effectively solving the problem that existing low-carbon decorative materials often fail to simultaneously meet the requirements for flexibility, abrasion resistance, flame retardancy, and water impermeability. Detailed Implementation
[0038] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0039] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indications will also change accordingly.
[0040] Furthermore, if the embodiments of this invention involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the use of "and / or" or "and / or" throughout the text includes three parallel solutions. For example, "A and / or B" includes solution A, solution B, or a solution where both A and B are satisfied simultaneously. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.
[0041] Flexible ceramic tile is a new type of environmentally friendly building decoration material. This material combines the advantages of traditional ceramic tiles and flexible decorative materials, featuring lightweight, flexibility, strong weather resistance, and ease of installation, making it suitable for both indoor and outdoor wall decoration. Currently, commercially available flexible ceramic tile materials have poor moisture regulation capabilities and high water absorption rates, making it difficult to meet the impermeability requirements of the flexible ceramic tile industry standard. Furthermore, prolonged exposure to moisture reduces the durability of flexible ceramic tile, thus shortening its service life. In addition, the flexibility, wear resistance, and flame retardancy of conventional flexible ceramic tile materials often fail to meet customer requirements. Therefore, developing a low-carbon decorative material that balances flexibility, wear resistance, flame retardancy, and impermeability is of great significance to the field of building decoration materials.
[0042] Currently, there is an oversupply of hemp stalks, with huge reserves worldwide. Hemp stalks are a renewable material; for example, the stems of hemp and flax are tough, rich in fiber, and possess excellent ecological properties. In the environmental field, hemp stalks can be used to make eco-friendly buildings, eco-friendly furniture, and eco-friendly flooring. Currently, hemp building materials mainly include hemp concrete and hemp building blocks. Hemp building materials are highly breathable, regulate humidity, prevent mold growth, and maintain suitable humidity levels. Hemp building materials are environmentally friendly and non-toxic, do not release toxins into indoor air, and also have antifungal effects.
[0043] Based on the above background, the present invention proposes a soft ceramic material made from hemp stalks. The raw materials of the soft ceramic material made from hemp stalks include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, curing agent, dispersant, film-forming aid, and waterproofing agent; wherein the mineral powder includes granite powder, quartz powder, and corundum powder.
[0044] In the technical solution of this invention, the raw materials for the soft ceramic material made from hemp stalks include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, and additives. The mineral powder includes granite powder, quartz powder, and corundum powder. The coupling agent is used to organically modify the surfaces of the alkali-modified hemp stalk powder, mineral powder, and inorganic filler, improving their compatibility with other organic materials. These powders modified by the coupling agent then undergo a cross-linking reaction under the combined action of the organophosphorus flame retardant, first emulsion, second emulsion, and additives to form a three-dimensional network structure, thus obtaining the soft ceramic material made from hemp stalks.
[0045] This invention uses alkali-modified hemp stalk powder, mineral powder, inorganic fillers, and organophosphorus flame retardants as main raw materials, and curing agents, dispersants, film-forming aids, and waterproofing agents as auxiliary agents. The addition of alkali-modified hemp stalk powder improves the flexibility, abrasion resistance, cigarette burn resistance, scratch resistance, and water impermeability of the flexible ceramic material. The addition of mineral powder serves as the main structural basis of the flexible ceramic material, providing hardness, strength, and abrasion resistance. The addition of granite powder improves the abrasion resistance, cigarette burn resistance, scratch resistance, and water impermeability of the flexible ceramic material. The addition of organophosphorus flame retardants not only improves flame retardancy but also enhances the abrasion resistance, cigarette burn resistance, and water impermeability of the flexible ceramic material. The addition of inorganic fillers improves the fire resistance, mechanical properties, and thermal stability of the material. Furthermore, the organophosphorus flame retardant and inorganic fillers together form a composite flame retardant, resulting in a better flame retardant effect compared to using only flame retardants or only inorganic materials. Using the raw materials for soft ceramic materials made from hemp stalks provided by this invention is beneficial for producing soft ceramic materials with good comprehensive performance, and solves the problem that existing low-carbon decorative materials cannot simultaneously meet the requirements for flexibility, wear resistance, flame retardancy and water impermeability.
[0046] It should be noted that in the technical solution of this invention, the first emulsion and the second emulsion are used to enhance the flexibility, elasticity, and adhesion of the soft ceramic material, enabling it to adapt to different application requirements; the curing agent is used to accelerate the cross-linking process between polymer chains, causing the material to transform from a liquid or semi-solid state to a solid state, thereby improving the mechanical properties of the material; the dispersant helps to ensure the uniform distribution of each raw material, thereby improving the quality and performance of the final soft ceramic material; the film-forming aid helps polymer particles form a continuous and uniform film, improving and optimizing the performance of the final coating or material, thereby improving the durability, flexibility, and waterproof performance of the material; the waterproofing agent can effectively prevent water from penetrating into the interior of the material, thereby avoiding problems such as expansion, deformation, mildew, or strength reduction caused by water absorption, and improving the waterproof performance and weather resistance of the material.
[0047] In an embodiment of the present invention, the raw materials for the soft ceramic material made from hemp stalks include the following components in parts by weight:
[0048] The composition includes: 70-150 parts alkali-modified hemp stalk powder, 180-220 parts granite powder, 500 parts quartz powder, 100 parts corundum powder, 50 parts inorganic filler, 30 parts organophosphorus flame retardant, 0.3-9 parts coupling agent, 2-10 parts first emulsion, 10-15 parts second emulsion, 0.1-0.4 parts curing agent, 0.1-0.4 parts dispersant, 0.1-0.4 parts film-forming aid, and 0.1-0.4 parts waterproofing agent.
[0049] Alkali-modified hemp stalk powder can improve the moisture regulation, flexibility, and scratch resistance of flexible ceramic materials. However, too much alkali-modified hemp stalk powder can cause internal stress concentration in the flexible ceramic due to its small mesh size, leading to cracking. Too little alkali-modified hemp stalk powder will result in insignificant performance improvement. Setting the dosage of alkali-modified hemp stalk powder within the above-mentioned range is beneficial for improving the stiffness and overall morphology of the material. Mineral powder, as the main structural basis of flexible ceramic materials, affects the hardness, strength, and wear resistance of the materials. Setting the dosage of mineral powder within the above-mentioned range ensures sufficient base material to achieve the required structural strength and stability. Furthermore, granite is a common acidic igneous rock with coarse grains. When the dosage is set within the above-mentioned range, the amount of emulsion used in the preparation of flexible ceramic materials is small, which can reduce costs while maintaining the performance of the flexible ceramic materials. Inorganic fillers, as halogen-free flame retardants and fillers, can improve the fire resistance, mechanical properties, and thermal stability of the materials. However, too little inorganic filler can lead to problems. Excessive use can lead to substandard flame retardancy, while excessive dosage increases costs. Furthermore, too much fine powder can increase internal stress, causing material cracking. Organophosphorus flame retardants not only improve flame retardancy but also enhance the wear resistance of flexible ceramic materials. Setting the dosage of organophosphorus flame retardants within the aforementioned range ensures that the flexible ceramic material meets flame retardancy requirements while controlling production costs. Appropriate amounts of silane coupling agents can improve the compatibility between inorganic and organic materials, increasing the degree of cross-linking between inorganic and organic macromolecules, thereby enhancing the overall performance of the flexible ceramic material. The first and second emulsions enhance the flexibility, elasticity, and adhesion of the flexible ceramic material, enabling it to adapt to different application needs. Setting the dosage of the first and second emulsions within the aforementioned range allows the use of composite emulsions to combine the advantages of both: the excellent wear resistance of polyurethane emulsions and the excellent adhesion of vinyl acetate-acrylic emulsions. Using these dosages within this range can reduce costs while meeting performance requirements. Considering the interactions between the materials, setting the raw materials in the above proportions results in flexible ceramic materials made from hemp stalks with good overall performance.
[0050] In an embodiment of the present invention, the alkali-modified hemp stalk powder is prepared according to the following steps:
[0051] Dry hemp stalks are soaked in an alkaline solution to obtain alkaline-treated hemp stalks. The alkaline-treated hemp stalks are then dried and pulverized to obtain alkali-modified hemp stalk powder.
[0052] After treating hemp stalks with an alkaline solution, the pectin, hemicellulose, and other gum substances in the stalks are removed, allowing the hemp fibers to be separated and purified. Simultaneously, the fibers become softer and smoother, increasing their flexibility and elasticity, while their rigidity and brittleness are correspondingly reduced, making them easier to process and use. Furthermore, alkaline treatment reduces the content of silica and waxy substances on the surface of the hemp stalks, increases surface polarity and surface energy, which enhances the interaction between the hemp stalks and other materials, improves the bonding performance between the hemp stalks and emulsions, and exposes more active sites, thus enhancing the activity of the hemp stalks.
[0053] In an embodiment of the present invention, an aqueous sodium hydroxide solution with a mass percentage concentration of 10% to 15% is used for alkali modification, and the mass ratio of the dried hemp stalks to the aqueous sodium hydroxide solution is 1:(5-10). Insufficient alkaline solution results in poor removal of pectin, hemicellulose, silica, and waxy substances from the hemp stalks; excessive alkaline solution may damage the original crystal structure of the hemp stalks, affecting the mechanical properties of the material. In one embodiment of the present invention, the aqueous sodium hydroxide solution has a mass percentage concentration of 15%.
[0054] In an embodiment of the present invention, the soaking time is 0.3 to 1 hour. Excessive soaking time may cause the original cellulose chains in the hemp stalks to break, affecting the mechanical properties of the material. In one embodiment of the present invention, the soaking time is set to 40 minutes.
[0055] In embodiments of the present invention, the soaking temperature is 50–80°C. Soaking at too low a temperature will prolong the soaking time, which is detrimental to removing impurities such as hemicellulose and pectin from the hemp stalks. Preferably, the soaking temperature is set to 50–60°C. In one embodiment of the present invention, the pressing temperature is 55°C.
[0056] In embodiments of the present invention, the particle size of the alkali-modified hemp stalk powder is 70 mesh to 500 mesh. Preferably, the particle size of the alkali-modified hemp stalk powder is set to 300 mesh to 400 mesh. Different particle sizes of the alkali-modified hemp stalk powder will affect the flexibility of the soft ceramic material. If the particle size is too coarse, it will affect the flexibility; if it is too fine, it will increase internal stress, causing it to crack, and if it is too fine, it will increase the difficulty of processing.
[0057] In an embodiment of the present invention, the fineness of the quartz powder is 200 mesh to 6000 mesh.
[0058] In an embodiment of the present invention, the fineness of the granite powder is 60 mesh to 100 mesh.
[0059] In an embodiment of the present invention, the fineness of the corundum powder is 60 mesh to 120 mesh.
[0060] Coarse-grained mineral powder can provide skeletal support, increasing the volume stability and compressive strength of flexible ceramic materials; fine-grained mineral powder helps fill voids, improving the density and surface quality of flexible ceramic materials. The technical solution of this invention, by precisely controlling the fineness of various mineral powders, ensures material strength while also considering its density and aesthetics.
[0061] In embodiments of the present invention, the inorganic filler includes at least one of modified aluminum hydroxide and modified magnesium hydroxide. The inclusion of at least one of modified aluminum hydroxide and modified magnesium hydroxide in the inorganic filler means that the inorganic filler can be any one of modified aluminum hydroxide and modified magnesium hydroxide, or two of them. The combined use of modified aluminum hydroxide and modified magnesium hydroxide results in a more effective flame-retardant soft ceramic material.
[0062] In embodiments of the present invention, the modified aluminum hydroxide and modified magnesium hydroxide are prepared by themselves, and the preparation steps of the modified aluminum hydroxide include:
[0063] 60g of aluminum hydroxide (300 mesh particle size, purchased from Yangzhou Dilan Co., Ltd., Jiangsu Province) and 1g of silane coupling agent KH550 were mixed at 60℃, and then a mixed solution of 10g water, 1g oxalic acid, and 50g ethanol was added dropwise to obtain modified aluminum hydroxide. Modification of aluminum hydroxide with a silane coupling agent can increase its dispersibility in inorganic powders and organically bind its surface, thereby enhancing its adhesion to organic emulsions.
[0064] The preparation steps of the modified magnesium hydroxide include:
[0065] 30g of magnesium hydroxide (300 mesh particle size, purchased from Yatai United Chemical Co., Ltd., Wuxi City, Jiangsu Province) and 0.5g of silane coupling agent KH550 were mixed at 60℃, followed by the addition of 10g of water, 1g of oxalic acid, and 50g of a mixed solution to carry out a coupling reaction, yielding modified magnesium hydroxide. Modification of magnesium hydroxide with a silane coupling agent can increase its dispersibility in inorganic powders and organically bind its surface, thereby enhancing its adhesion to organic emulsions.
[0066] In embodiments of the present invention, the first emulsion comprises a polyurethane emulsion, and the second emulsion comprises at least one selected from vinyl acetate-acrylic emulsion, pure acrylic emulsion, ethylene-vinyl acetate copolymer emulsion, styrene-acrylic emulsion, and vinyl acetate emulsion. The first emulsion can enhance the mechanical strength and wear resistance of the material; the second emulsion has good bonding properties and can enhance the bonding effect of the raw materials. By using two emulsions simultaneously, with the second emulsion as the base and introducing a first emulsion having multiple glass transition temperatures, the second emulsion can have a greater difference in temperature adaptability, thereby better adapting to a wide range of temperature changes and improving the weather resistance of the resulting soft ceramic material.
[0067] In embodiments of the present invention, the organophosphorus flame retardant includes a phosphate ester flame retardant. Adding an organophosphorus flame retardant not only improves flame retardant properties but also enhances the wear resistance of flexible ceramic materials.
[0068] In embodiments of the present invention, the coupling agent includes at least two of titanate coupling agents, aluminate coupling agents, and silane coupling agents. Coupling agents can improve the compatibility between polymeric materials and inorganic powders, enhance interfacial adhesion, and thus improve the performance of soft ceramic materials. Using multiple types of coupling agents simultaneously is more effective than using a single coupling agent. For example, the hydrophilic groups in silane coupling agent KH570 and the lipophilic groups in titanate coupling agents, under certain component ratios, achieve a balance between their hydrophilic and lipophilic values, resulting in a synergistic effect. In one embodiment of the present invention, titanate coupling agents, aluminate coupling agents, and silane coupling agents are used simultaneously as coupling agents.
[0069] In embodiments of the present invention, the curing agent includes any one of aziridine curing agents, polycarbodiimide curing agents, and isocyanate curing agents. The curing agent can accelerate the cross-linking process between polymer chains, causing the material to transform from a liquid or semi-solid state to a solid state, thereby improving the material's mechanical properties, such as hardness, strength, and chemical resistance. The curing agent in the technical solution of the present invention is a water-based curing agent. Utilizing the water-based curing agent to participate in the cross-linking and curing of water-based emulsions can improve the material's heat resistance, abrasion resistance, and mechanical strength.
[0070] In embodiments of the present invention, the dispersant comprises a sodium polycarboxylate dispersant. Sodium polycarboxylate dispersants have low foaming properties and stable slurry viscosity, which can improve the flowability of coatings. In one embodiment of the present invention, the dispersant is dispersant SN 5040.
[0071] In embodiments of the present invention, the film-forming aid includes at least one selected from 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate (alcohol ester 12), benzyl alcohol, and dibutyl phthalate. The film-forming aid helps form a smooth, uniform surface film, increases the appearance quality of the material, ensures a good film layer can be formed on the material surface, and enhances aesthetics and functionality.
[0072] In embodiments of the present invention, the waterproofing agent includes an organosilicon-based waterproofing agent. The waterproofing agent can improve the waterproof performance of the material and reduce the impact of moisture on the material.
[0073] This invention proposes a method for preparing a flexible ceramic material using hemp stalks. The method involves using the raw materials for preparing the flexible ceramic material made from hemp stalks, wherein the raw materials include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, curing agent, dispersant, film-forming aid, and waterproofing agent; wherein the mineral powder includes granite powder, quartz powder, and corundum powder.
[0074] The method for preparing the soft ceramic material made from hemp stalks includes the following steps:
[0075] The coupling agent is dispersed in an alcohol solution to obtain a coupling agent solution; alkali-modified hemp stalk powder, mineral powder and inorganic filler are mixed to obtain a mixed powder; the coupling agent solution is added to the mixed powder to obtain a first mixture;
[0076] A curing agent, dispersant, film-forming aid, and water are mixed to obtain a second mixture. Then, an organophosphorus flame retardant, a first emulsion, a second emulsion, and a waterproofing agent are added to the second mixture to obtain a third mixture.
[0077] The first mixture and the third mixture are mixed to obtain a slurry;
[0078] The slurry is poured into a mold, pressed into shape, dried, and demolded to obtain the soft ceramic material made from hemp stalks.
[0079] Using the above preparation method, inorganic powder is first organicated by the action of silane to enhance the adhesion between it and the polymer. Then, the modified components are mixed with the emulsion to undergo a cross-linking reaction, forming a three-dimensional network structure at a certain temperature.
[0080] In embodiments of the present invention, the compression molding pressure is 3–15 MPa. Exemplarily, the compression molding pressure can be 3 MPa, 5 MPa, 7 MPa, 10 MPa, 12 MPa, or 15 MPa. In one embodiment of the present invention, the compression molding pressure is 10 MPa.
[0081] In embodiments of the present invention, the pressing temperature is 50–70°C. Exemplarily, the pressing temperature can be 50°C, 55°C, 60°C, 65°C, or 70°C. In one embodiment of the present invention, the pressing temperature is 60°C.
[0082] In embodiments of the present invention, the pressing and molding time is 0.3 to 0.5 hours. Exemplarily, the pressing and molding time can be 0.3 hours, 0.4 hours, or 0.5 hours. In one embodiment of the present invention, the pressing and molding time is 0.4 hours.
[0083] In embodiments of the present invention, the drying temperature is 40–80°C. Preferably, the drying temperature is 50–70°C. Exemplarily, the drying temperature may be 50°C, 55°C, 60°C, 65°C, or 70°C. In one embodiment of the present invention, the drying temperature is 60°C.
[0084] In embodiments of the present invention, the drying time is 4–16 hours. Preferably, the drying time is 5–12 hours. The pressing and molding time can be 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, or 12 hours. In one embodiment of the present invention, the drying time is 8 hours.
[0085] In embodiments of the present invention, the curing agent includes any one of polyamides, isopropionic acid esters, formaldehyde, aziridine, and polycarbodiimides. The curing agent accelerates the cross-linking process between polymer chains, causing the material to transform from a liquid or semi-solid state to a solid state, thereby improving the material's mechanical properties, such as hardness, strength, and chemical resistance. The curing agent in the technical solution of this invention is a water-based curing agent. Utilizing the water-based curing agent to participate in the cross-linking and curing of water-based emulsions can improve the material's heat resistance, abrasion resistance, and mechanical strength.
[0086] The technical solution of the present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are only used to explain the present invention and are not intended to limit the present invention.
[0087] In the following embodiments and comparative examples:
[0088] The hemp stalks are hemp (industrial hemp) stems, purchased from Yunnan Hanmusen Biotechnology; the straw was also purchased from Yunnan Hanmusen Biotechnology.
[0089] The quartz powder was purchased from Runjia Quartz Sand Factory, with a particle size of 400 mesh; the granite powder was purchased from Yunfu Stone Factory, with a particle size of 60-100 mesh; and the corundum powder was purchased from Gongyi Chaoyue Filter Material Factory, with a particle size of 60 mesh.
[0090] The phosphate ester flame retardant was purchased from Sichuan Longmang Group's APP flame retardant (FR-1000 series);
[0091] The titanate coupling agent was purchased from Nanjing Shuguang Chemical KR-38S titanate coupling agent (dioctyl pyrophosphate titanate).
[0092] The aluminate coupling agent was purchased from Anhui Sibao Organosilicon New Materials Co., Ltd.
[0093] The silane coupling agent was purchased from Nanjing Shuguang Chemical Co., Ltd.
[0094] The polyurethane emulsion was F0410, purchased from Shenzhen Yoshida Chemical Co., Ltd.
[0095] The acrylic emulsion CR-508 was purchased from Jiangsu Sunrise Chemical Co., Ltd.
[0096] The curing agent is polycarbodiimide, purchased from Novick Chemicals;
[0097] The dispersant was SN5040, purchased from Sannopco.
[0098] The film-forming aid is alcohol ester 12, purchased from Nanjing Weier Chemical Co., Ltd., product model WE-12;
[0099] The waterproofing agent is an organosilicone fluorine-based waterproofing agent, purchased from Guangzhou Yuchuang Company as model YC265 waterproofing agent.
[0100] Example 1
[0101] A method for preparing alkali-modified hemp stalk powder includes the following steps:
[0102] 80g of dried hemp stalks were soaked in a 15% sodium hydroxide aqueous solution at 55℃ (the mass ratio of dried hemp stalks to alkali solution was 1:10) for 40 minutes to obtain alkali-treated hemp stalks. The alkali-treated hemp stalks were then dried at 200℃ and pulverized to obtain alkali-modified hemp stalk powder. The particle size of the alkali-modified hemp stalk powder was 300 mesh.
[0103] Example 2
[0104] A method for preparing a soft ceramic material using hemp stalks includes the following steps:
[0105] (1) Weigh the following raw materials: 80g of alkali-modified hemp stalk powder, 200g of granite powder, 500g of quartz powder, 100g of corundum powder, 30g of modified aluminum hydroxide, 20g of modified magnesium hydroxide, 30g of phosphate ester flame retardant, 1g of titanate coupling agent, 1g of aluminate coupling agent, 1g of silane coupling agent, 5g of polyurethane emulsion, 12g of vinyl acetate emulsion, 1g of polycarbodiimide, 1g of SN 5040 dispersant, 1g of alcohol ester 12, 1g of organosilicon waterproofing agent, 10g of alcohol solution (obtained by mixing anhydrous ethanol and water at a mass ratio of 7:3), and 100g of water;
[0106] (2) Disperse titanate coupling agent, aluminate coupling agent and silane coupling agent in alcohol solution to obtain coupling agent solution; mix alkali modified hemp stalk powder, granite powder, quartz powder, corundum powder, modified aluminum hydroxide and modified magnesium hydroxide to obtain mixed powder; add the coupling agent solution dropwise to the mixed powder to obtain first mixture;
[0107] (3) Mix polycarbodiimide, SN 5040 dispersant, alcohol ester 12 and water to obtain a second mixture. Then add phosphate flame retardant, polyurethane emulsion, vinyl acetate emulsion and silicone waterproofing agent to the second mixture and stir for 30 minutes to obtain a third mixture.
[0108] (4) Mix the first mixture and the third mixture and stir for 15 minutes to obtain a slurry;
[0109] (5) Pour the slurry into a mold and press it into shape (parameters: pressure is 10MPa, temperature is 60℃, time is 0.4h), then place it at 60℃ to dry for 8h, and demold to obtain the soft porcelain material made from hemp stalks.
[0110] Example 3
[0111] The difference compared to Example 2 is that the amount of alkali-modified hemp stalk powder used is 10g.
[0112] Example 4
[0113] The difference compared to Example 2 is that the amount of alkali-modified hemp stalk powder used is 150g.
[0114] Example 5
[0115] The difference compared to Example 2 is that the particle size of the alkali-modified hemp stalk powder is 70 mesh.
[0116] Example 6
[0117] The difference compared to Example 2 is that the particle size of the alkali-modified hemp stalk powder is 500 mesh.
[0118] Example 7
[0119] The difference compared to Example 2 is that the amount of granite powder used is 20g.
[0120] Example 8
[0121] The difference compared to Example 2 is that the amount of granite powder used is 220g.
[0122] Example 9
[0123] Compared with Example 2, the difference lies in the following amounts: titanate coupling agent 0.1g, aluminate coupling agent 0.1g, silane coupling agent 0.1g, polyurethane emulsion 2g, vinyl acetate-acrylic emulsion 10g, polycarbodiimide 0.1g, SN 5040 dispersant 0.1g, alcohol ester 12 0.1g, waterproofing agent 0.1g, alcohol solution 40g, and water 100g.
[0124] Example 10
[0125] Compared with Example 2, the difference lies in the amount of titanate coupling agent (4g), aluminate coupling agent (4g), silane coupling agent (4g), polyurethane emulsion (10g), vinyl acetate emulsion (15g), polycarbodiimide (4g), SN 5040 dispersant (4g), alcohol ester 12 (4g), waterproofing agent (4g), alcohol solution (40g), and water (90g).
[0126] Comparative Example 1
[0127] The difference compared to Example 2 is that the amount of alkali-modified hemp stalk powder used is 0.
[0128] Comparative Example 2
[0129] The difference compared to Example 2 is that the amount of granite powder used is 0.
[0130] Comparative Example 3
[0131] The difference compared to Example 2 is that the amount of phosphate flame retardant used is 0.
[0132] Comparative Example 4
[0133] Compared with Example 2, the difference is that an equal amount of unmodified hemp stalks was used instead of alkali-modified hemp stalk powder.
[0134] Comparative Example 5
[0135] Compared with Example 2, the difference is that an equal amount of alkali-modified straw powder is used instead of alkali-modified hemp stalk powder, and the preparation method of the alkali-modified straw powder is the same as that in Example 1.
[0136] Performance testing
[0137] The flexibility, abrasion resistance (load 5N), cigarette burn resistance, scratch resistance, flame retardancy, and water impermeability of the soft ceramic materials prepared in Examples 2-9 and Comparative Examples 1-5 were tested. The test results are shown in Table 1. The test methods are as follows:
[0138] Flexibility: The reference criteria for judging the absence of cracks or fractures refer to JC / T864-2023; where the number of cracks in a 20cm×20cm area is 0, it is judged as "no obvious cracks"; the number of cracks is in the range of 1 to 10, it is judged as "minor cracks"; the number of cracks is in the range of 10 to 20, it is judged as "a small number of cracks"; and the number of cracks is in the range of 20 to 40, it is judged as "a certain amount of cracks".
[0139] Abrasion resistance (g / 100r): Tested according to GB / T15036.2-2011.
[0140] Resistance to cigarette burns: Tested according to standard HG / T3747.1-2011.6.5.
[0141] Surface scratch resistance: Visual inspection, the judgment criteria are as follows: Level 5: No scratches visible to the naked eye within a 20cm×20cm area; Level 4: Very fine scratches visible under specific angles of light, not obvious under normal viewing angle; Level 3: Clear scratches visible under normal viewing angle, but not penetrating the surface coating or substrate; Level 2: Scratches with obvious depth, possibly exposing part of the underlying material and affecting the appearance; Level 1: Deep and wide scratches that penetrate the surface and cause significant damage to the material properties or appearance.
[0142] Flame retardancy: Tested in accordance with GB / T 14833-2020.
[0143] Impermeability: The test shall be conducted in accordance with GB / T328.10. The judgment criteria are as follows: No leakage: No water droplets seep out from the surface of the specimen after 30 minutes under the specified pressure (0.3MPa); Slight leakage: Water droplets condense during the pressure holding period but do not form water flow, and there is no residue after wiping dry after the test is stopped; Severe leakage: Water flow occurs or the pressure cannot be maintained, and the impermeability is deemed unqualified.
[0144] Table 1 Performance test results of Examples 2-9 and Comparative Examples 1-5
[0145]
[0146]
[0147] The following conclusions can be drawn from Table 1:
[0148] (1) Example 2 has the best overall performance. Using the raw materials and preparation method of Example 2 is beneficial to improving the overall performance of soft ceramic materials.
[0149] (2) The test results of Example 2, Comparative Example 1 and Comparative Examples 4-5 show that the test results of flexibility, abrasion resistance, cigarette burn resistance, surface scratch resistance and water impermeability of Example 2 are all better than those of Comparative Example 1. It can be seen that adding alkali-modified hemp stalks is beneficial to the flexibility, cigarette burn resistance, surface scratch resistance and water impermeability of soft porcelain materials. The test results of flexibility, abrasion resistance, cigarette burn resistance, surface scratch resistance and water impermeability of Example 2 are all better than those of Comparative Examples 4-5. This shows that compared with unmodified hemp stalk powder or alkali-modified straw powder, the use of alkali-modified hemp stalk powder is more beneficial to improving the flexibility, abrasion resistance, cigarette burn resistance, surface scratch resistance and water impermeability of soft porcelain materials.
[0150] (3) The test results of Examples 2-4 show that the flexibility and wear resistance test results of Example 2 are better than those of Examples 3-4, indicating that too little or too much alkali-modified hemp stalk powder will reduce the effect of alkali-modified hemp stalk powder on improving the flexibility or wear resistance of soft porcelain materials; the cigarette burn resistance, scratch resistance, flame retardancy and water impermeability of Examples 2-3 are better than those of Example 4, indicating that excessive alkali-modified hemp stalk powder will reduce the effect of alkali-modified hemp stalk powder on improving the cigarette burn resistance, scratch resistance, flame retardancy and water impermeability of soft porcelain materials.
[0151] (4) As can be seen from the test results of Examples 2 and 5-6, the test results of flexibility, wear resistance, cigarette burn resistance and flame retardancy are all greater in Example 2 than in Example 5-6. This indicates that if the alkali-modified hemp stalk powder particles are too large (Example 5) or too small (Example 6), the improvement effect of alkali-modified hemp stalk powder on the flexibility, wear resistance, cigarette burn resistance and flame retardancy of soft porcelain materials will be worse.
[0152] (5) The test results of Example 2 and Comparative Example 2 show that adding granite powder is beneficial to improving the wear resistance, cigarette burn resistance, scratch resistance and water impermeability of the soft ceramic material. Furthermore, the test results of Example 2 and Examples 7-8 show that too much or too little granite powder will result in a worse improvement effect on the flexibility, wear resistance, cigarette burn resistance and scratch resistance of the soft ceramic material.
[0153] (6) As can be seen from the test results of Example 2 and Comparative Example 3, adding an appropriate amount of phosphate flame retardant is beneficial to improving the wear resistance, cigarette burn resistance, flame retardancy and water impermeability of soft ceramic materials.
[0154] The above description is merely an exemplary embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention under the technical concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.
Claims
1. A raw material for a flexible ceramic material made from hemp stalks, characterized in that, The raw materials for the soft ceramic material made from hemp stalks include alkali-modified hemp stalk powder, mineral powder, inorganic filler, organophosphorus flame retardant, coupling agent, first emulsion, second emulsion, curing agent, dispersant, film-forming aid, and waterproofing agent; wherein the mineral powder includes granite powder, quartz powder, and corundum powder.
2. The raw material for the soft ceramic material made from hemp stalks as described in claim 1, characterized in that, The raw materials for the soft ceramic material made from hemp stalks include the following components in parts by weight: The composition includes: 70-150 parts alkali-modified hemp stalk powder, 180-220 parts granite powder, 500 parts quartz powder, 100 parts corundum powder, 50 parts inorganic filler, 30 parts organophosphorus flame retardant, 0.3-9 parts coupling agent, 2-10 parts first emulsion, 10-15 parts second emulsion, 0.1-0.4 parts curing agent, 0.1-0.4 parts dispersant, 0.1-0.4 parts film-forming aid, and 0.1-0.4 parts waterproofing agent.
3. The raw material for the soft ceramic material made from hemp stalks as described in claim 1, characterized in that, The alkali-modified hemp stalk powder is prepared according to the following steps: Dry hemp stalks are soaked in an alkaline solution to obtain alkaline-treated hemp stalks. The alkaline-treated hemp stalks are then dried and pulverized to obtain alkali-modified hemp stalk powder.
4. The raw material for the soft ceramic material made from hemp stalks as described in claim 3, characterized in that, The alkaline solution is a 10%–15% sodium hydroxide aqueous solution, and the mass ratio of the dried hemp stalks to the alkaline solution is 1:(5–10); and / or, The soaking time is 0.3–1 hour; and / or, The soaking temperature is 50–80°C.
5. The raw material for the soft ceramic material made from hemp stalks as described in claim 1, characterized in that, The alkali-modified hemp stalk powder has a particle size of 300-400 mesh; and / or, The quartz powder has a fineness of 200 mesh to 6000 mesh; and / or, The granite powder has a fineness of 60 mesh to 100 mesh; and / or, The fineness of the corundum powder is 60 mesh to 120 mesh.
6. The raw material for the soft ceramic material made from hemp stalks as described in claim 1, characterized in that, The inorganic filler includes at least one of modified aluminum hydroxide and modified magnesium hydroxide; and / or, The first emulsion comprises a polyurethane emulsion, and the second emulsion comprises at least one selected from vinyl acetate-acrylic emulsion, pure acrylic emulsion, ethylene-vinyl acetate copolymer emulsion, styrene-acrylic emulsion, and vinyl acetate emulsion; and / or, The organophosphorus flame retardant includes phosphate ester flame retardants; and / or, The coupling agent includes at least two of titanate coupling agents, aluminate coupling agents, and silane coupling agents; and / or, The curing agent includes any one of aziridine curing agents, polycarbodiimide curing agents, and isocyanate curing agents; and / or, The dispersant includes sodium polycarboxylate type dispersants; and / or, The film-forming aid includes at least one selected from 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, benzyl alcohol, and dibutyl phthalate; and / or... The waterproofing agent includes silicone-based waterproofing agents.
7. A method for preparing a soft ceramic material using hemp stalks, characterized in that, The method for preparing the soft ceramic material made from hemp stalks, using the raw materials described in any one of claims 1 to 6, comprises the following steps: The coupling agent is dispersed in an alcohol solution to obtain a coupling agent solution; alkali-modified hemp stalk powder, mineral powder, and inorganic filler are mixed to obtain a mixed powder; the coupling agent solution is added to the mixed powder to obtain a first mixture; A curing agent, dispersant, film-forming aid, and water are mixed to obtain a second mixture. Then, an organophosphorus flame retardant, a first emulsion, a second emulsion, and a waterproofing agent are added to the second mixture to obtain a third mixture. The first mixture and the third mixture are mixed to obtain a slurry; The slurry is poured into a mold, pressed into shape, dried, and demolded to obtain the soft ceramic material made from hemp stalks.
8. The method for preparing soft ceramic material using hemp stalks as described in claim 7, characterized in that, The pressing pressure is 3–15 MPa; and / or, The pressing temperature is 50–70°C; and / or, The pressing and molding time is 0.3 to 0.5 hours.
9. The method for preparing soft ceramic material using hemp stalks as described in claim 7, characterized in that, The drying temperature is 40–80°C; and / or, The drying time is 4 to 16 hours.
10. A soft ceramic material made from hemp stalks, characterized in that, The soft ceramic material made from hemp stalks is prepared according to the method for preparing soft ceramic material made from hemp stalks according to any one of claims 7 to 9.