A single-component formaldehyde-free setting agent for mineral wool and a method for determining its pot life.

Abstract

This application provides a single-component formaldehyde-free styling agent specifically for mineral wool and a method for detecting its shelf life. The formaldehyde-free styling agent uses a formaldehyde-free binder as the matrix component, mixed with a compatible reactive silane coupling agent. Optionally, it also includes water-repellent agents and dust-proofing oils, etc., to produce a mineral wool product styling agent with long-term stability. This styling agent not only avoids the use of formaldehyde at the source, meeting environmental protection requirements, but also has a shelf life of more than 6 months, or even more than 12 months. This changes the traditional industry situation where styling agents need to be prepared on demand, providing a "ready-to-use" styling agent, realizing the mass production of single-component styling agents, thereby ensuring the quality stability of the styling agent. The detection method provided in this application can realize laboratory testing of the shelf life of mineral wool styling agents without the need for production line testing.

Description

Technical Field

[0001] This invention belongs to the field of polymer chemical materials, specifically relating to a single-component formaldehyde-free setting agent for mineral wool and a method for determining its pot life. Background Technology

[0002] Mineral wool typically includes rock wool, glass wool, and slag wool. Due to its lightweight, good thermal insulation, low thermal conductivity, strong heat resistance, sound insulation, waterproofing, chemical stability, acid and alkali resistance, and corrosion resistance, mineral wool has become a new type of lightweight insulation material. In the mineral wool industry, shaping agents are typically used to bind loose mineral wool and shape it into boards, felts, or other mineral wool products with predetermined shapes, thereby giving the mineral wool products a predetermined strength.

[0003] For a long time, the base components of the sizing agents used in the mineral wool industry have mainly included urea-formaldehyde resin, phenolic resin, or melamine resin (hereinafter referred to as "trialdehyde resin"). Among them, phenolic resin-based sizing agents are used in the largest quantities, with approximately 600,000 tons of phenolic resin consumed annually in the mineral wool industry. Since phenolic resin inevitably contains a large amount of formaldehyde, the main raw material for its preparation, and formaldehyde is a Group 1 carcinogen, the use of phenolic resin-based sizing agents poses significant potential health and environmental hazards to both mineral wool producers and users.

[0004] As the country further tightens its environmental regulations, mineral wool producers using traditional setting agents are subject to strict controls or even production shutdowns due to the large amounts of formaldehyde and phenol wastewater they generate. Therefore, the mineral wool industry urgently needs an environmentally friendly and safe setting agent to replace traditional setting agents.

[0005] In addition, the sizing agents used in mineral wool typically require the addition of auxiliaries such as silane coupling agents, water-repellent agents, and dust-proof oils. Among these, silane coupling agents are essential for most mineral wool products, used to improve the bonding strength between mineral wool fibers, especially the wet strength under high temperature and humidity, thereby improving the water vapor resistance and aging resistance of mineral wool products. Water-repellent agents are added to most high-end mineral wool products, mainly including dimethyl silicone oil or modified silicone oil, etc., whose function is to repel water and moisture, giving the surface of mineral wool products a "lotus leaf" hydrophobic and moisture-proof effect, thereby preventing the thermal insulation performance of mineral wool products from decreasing due to water and moisture absorption. Dust-proof oil is an oil-based auxiliary agent made from mineral base oil, corn oil, rapeseed oil, and their combinations, used to improve the flexibility of mineral wool fibers, making it less likely for mineral wool fibers to break and scatter during the cutting process, thereby reducing dust generated during production and use.

[0006] Typically, silane coupling agents, water-repellent agents, and dust-proofing oils are prepared on-site rather than being directly added to phenolic resins or other formaldehyde-free setting agents to create single-component formaldehyde-free setting agents. The main reasons for this are:

[0007] 1. Phenolic resin itself has poor stability. In high-temperature environments, such as 30℃~40℃, its applicable period is only 15-45 days, making it unsuitable for use as a single-component formaldehyde-free setting agent.

[0008] 2. Since the phenolic resin stock solution contains a large amount of free formaldehyde, it is usually necessary to add additives such as urea and ammonia that have the function of absorbing formaldehyde. However, after adding the additives, the stability of the setting agent is further weakened in high temperature environment, such as 30℃~40℃, and the applicable period is shortened to only 2-10 days.

[0009] 3. Phenolic resin also needs to be used with accelerators such as ammonium sulfate to reduce the curing temperature. After adding ammonium sulfate curing agent, the pot life will be further shortened to 4h-8h in high temperature environment, such as 30℃~40℃.

[0010] 4. Phenolic resins are alkaline. When coupling agents such as KH550 are added to phenolic resin systems, they will rapidly hydrolyze, leading to polycondensation failure. Therefore, commonly used phenolic resin coupling agents cannot be used to prepare single-component formaldehyde-free shaping agents.

[0011] 5. Commonly used water-repellent agents and dust-proofing oils are usually made into water-based emulsions. Since phenolic resin is used as the sizing agent matrix, the added additives are basically prepared on the spot. Therefore, water-repellent agents and dust-proofing oils are also prepared on the spot.

[0012] Traditional methods of formulating and fixing agents have at least the following problems:

[0013] 1. The setting agent should be used immediately after preparation. If the production line is temporarily shut down, the setting agent may become ineffective due to prolonged storage, which not only reduces the flexibility of continuous production but also increases the changeover cost for the manufacturer.

[0014] 2. Each time the fixing agent is prepared, it is necessary to add auxiliary agents, which not only results in low material preparation efficiency but also high labor costs;

[0015] 3. The amount of each of the additives is relatively small, and operators are prone to errors during the preparation process, which can cause fluctuations in the quality of the setting agent and lead to unstable quality of mineral wool products.

[0016] 4. Mineral wool product production lines require a large number of auxiliary agent distribution equipment and pipelines, increasing equipment investment costs;

[0017] 5. Frequent weighing and preparation of various additives can easily lead to cumulative material loss.

[0018] Among existing formaldehyde-free setting agent patents, US5661213 discloses a curable aqueous composition comprising a polymeric polyacid polyol and a phosphorus-containing accelerator. This composition can be used as a formaldehyde-free binder in heat-resistant nonwoven fabrics such as those made of glass fiber. CN102363721A discloses a carbohydrate component consisting of one or more monosaccharides or disaccharides and oligosaccharides having at least three sugar groups, a polymeric polyacid, and a bleaching agent. The carbohydrates provide a curable binder capable of providing a thermosetting material with a light or white color and acceptable physical properties. However, none of the above-disclosed compositions or setting agents mention how to apply them to the mineral wool industry. CN101248151A discloses an aqueous binder for inorganic fibers that is formaldehyde-free, has excellent strength, and is suitable for use under weakly acidic to weakly alkaline conditions. However, it does not mention the preparation of a single-component setting agent, and the application method of the product remains the traditional on-the-spot preparation method.

[0019] For the reasons mentioned above, the mineral wool industry urgently needs to develop a single-component formaldehyde-free setting agent that differs from the existing phenolic resin process in order to solve the environmental and process problems of existing phenolic resins.

[0020] Furthermore, based on the total weight of mineral wool products, the weight ratio of the sizing agent is generally only 1.5wt%-10wt%, while the majority is mineral wool fiber. Therefore, in terms of the overall performance of mineral wool products, the quality of mineral wool fiber has a significant impact on the quality of the mineral wool products. However, existing methods for evaluating the quality of mineral wool products make it difficult to separate the sizing agent from the mineral wool fiber and then evaluate the quality of the sizing agent and mineral wool fiber separately. The quality of mineral wool fiber is greatly affected by the production process, resulting in unstable product quality. Therefore, in the process of switching to formaldehyde-free sizing agents, simply evaluating the quality of the mineral wool product cannot accurately assess the quality of the sizing agent, leading to increased testing costs. In addition, the mineral wool industry is a continuous, large-scale production industry, typically with an output of 20,000 tons / year per production line. Currently, there are no small-scale or pilot-scale mineral wool production lines in China, requiring each test to be conducted directly on a large-scale production line, further increasing the testing and switching costs for single-component formaldehyde-free sizing agents.

[0021] For the reasons mentioned above, it is of great significance to evaluate the pot life of fixatives using laboratory methods, as this can greatly reduce testing costs and switching costs. Summary of the Invention

[0022] To address the problems existing in the prior art, the applicant, through dedicated research, discovered that by using a formaldehyde-free adhesive as the base component and mixing it with compatible reactive silane coupling agents, water-repellent agents, and dust-proofing oils, a mineral wool product setting agent with long-term stability can be prepared. This setting agent not only avoids the use of formaldehyde at the source, meeting environmental protection requirements, but also has a usable period of more than 6 months. This changes the traditional industry practice of setting agents requiring on-the-spot preparation, providing a "ready-to-use" setting agent and enabling the mass production of single-component setting agents, thereby ensuring the quality stability of the setting agent.

[0023] In addition, this application provides a laboratory test method for determining the shelf life of a sizing agent, making it possible to evaluate the quality of mineral wool sizing agents in the laboratory, effectively reducing testing and switching costs.

[0024] The purpose of this application is to provide the following aspects:

[0025] In a first aspect, this application provides a single-component formaldehyde-free styling agent specifically for mineral wool, wherein, based on 100% solid content, the single-component formaldehyde-free styling agent comprises the following components in the indicated weight ratios:

[0026] 100 parts by weight of formaldehyde-free adhesive, wherein the formaldehyde-free adhesive is a non-trialdehyde resin that does not use formaldehyde as a direct raw material;

[0027] 0.1-5 parts by weight of a compatible reactive silane coupling agent;

[0028] One part by weight is calculated based on 1 kg.

[0029] Preferably, the pH of the single-component formaldehyde-free hairspray is 0.0–7.0, more preferably 2.5–5.5, and even more preferably 3.0–5.0. The applicant has found that within the above pH range, the single-component formaldehyde-free hairspray has a long pot life.

[0030] In this application, the formaldehyde-free adhesive is specifically a non-trialdehyde resin that does not use formaldehyde as a direct raw material, mainly including water-soluble thermosetting polyacrylate formaldehyde-free adhesive and water-soluble thermosetting bio-based formaldehyde-free adhesive.

[0031] The applicant has discovered that the two formaldehyde-free adhesives mentioned above are completely miscible with water in any proportion. Using the two formaldehyde-free adhesives as matrix components can keep the formaldehyde-free setting agent system in an acidic or weakly acidic state, so that compatible reactive silane coupling agents such as KH550 can remain stable in the formaldehyde-free adhesives and are not easily decomposed. Furthermore, the single-component formaldehyde-free setting agent is not easy to mold or deteriorate, and its service life can be greater than 6 months.

[0032] In this application, the water-soluble thermosetting polyacrylate formaldehyde-free binder comprises 60wt%-90wt% of unsaturated carboxylic acid oligomers and 10wt%-40wt% of polyols.

[0033] In this application, the solid content of the unsaturated carboxylic acid oligomer is 30wt%-60wt%, and the pH value is 2.0-4.0.

[0034] Furthermore, the unsaturated carboxylic acid oligomer can be obtained by polymerization of alkenyl unsaturated carboxylic acid monomers, or by copolymerization of carboxyl-free vinyl unsaturated monomers with alkenyl unsaturated carboxylic acid monomers.

[0035] Specifically, the alkenyl unsaturated carboxylic acid monomer may include one or more of the following: acrylic acid, methacrylic acid, crotonic acid, fumaric acid, maleic acid, 2-methylmaleic acid, itaconic acid, 2-methylitaconic acid, α-β-methyleneglutaric acid, monoalkyl maleate, monoalkyl fumaric acid, maleic anhydride, acrylic anhydride, hydrogen phthalate [β-(meth)acryloyloxyethylene] ester, hydrogen maleate [β-(meth)acryloyloxyethylene] ester, and hydrogen succinate [β-(meth)acryloyloxyethylene] ester.

[0036] Preferably, the alkenyl unsaturated carboxylic acid monomer is acrylic acid or methacrylic acid, wherein the number average molecular weight of the acrylic acid or methacrylic acid is 500-30000, preferably 800-10000, more preferably 1000-5000. In particular, the number average molecular weight can be determined using gel permeation chromatography (GPC).

[0037] Optionally, the carboxyl-free vinyl unsaturated monomer is preferably free of formaldehyde release during heat curing, and preferably selected from one or more of acrylate monomers, vinyl monomers, amide monomers, aliphatic unsaturated hydrocarbons, styrene monomers, vinyl ester monomers, acrylonitrile, and glycidyl (meth)acrylate.

[0038] In particular, since both N-hydroxymethyl (meth)acrylamide and methyl-N-hydroxymethyl (meth)acrylamide release formaldehyde upon heating due to cross-linking reactions, the use of these two raw materials should be avoided.

[0039] In this application, a catalyst may also be used to prepare the unsaturated carboxylic acid oligomers, and the catalyst may include hypophosphite, etc.

[0040] In this application, the polyol is a compound having two or more hydroxyl groups, specifically including alcohols with two or more hydroxyl groups, alkanolamine polyols, and addition polymers of alcohols with two or more hydroxyl groups.

[0041] Optionally, the alcohol compound having two or more hydroxyl groups may be selected from 1,2-ethylene glycol, 1,3-propanediol, diethylene glycol, 1,4-butanediol, 1,2,3-cyclohexanetriol, 1,2,4-butanetriol, 1,2,3-butanetriol, 1,2,5-pentanetriol, glycerol, glycerol polyether polyol, 2,2-dimethyl-1,3-propanediol, 2-butyl-2-ethyl-1,3-propanediol, 1,3-butanediol, 1,4-butanediol, 2-methyl-2,4-butanediol, 1,5-pentanediol, 3-methyl-1,5-pentanediol, 2-methyl-2,4-pentanediol, 1, 6-Hexanediol, 1,4-cyclohexanediol, 2-ethyl-1,3-hexanediol, 2-hydroxymethyl-2-methyl-1,3-propanediol, 2-ethyl-2-hydroxymethyl-2-methyl-1,3-propanediol, 1,2,6-hexanetriol, 2,2-dihydroxymethyl-2,3-propanediol, pentaerythritol, trimethylolpropane, glucose, fructose, sorbitol, sucrose, mannitol, maltose, glucose, resorcinol, catechol, pyrogallol, 1,2-ethylenediol dimer, 1,2-ethylenediol trimer, 1,2-propanediol, 1,2-propanediol dimer or 1,2-propanediol trimer, etc.

[0042] In this application, the alkanolamine polyol includes ethanolamine, isopropanolamine, diethanolamine, diisopropanolamine, or triethanolamine.

[0043] Furthermore, the applicant unexpectedly discovered that the introduction of the polyol component in this application further improves the stability of the setting agent and extends its pot life. Without being limited to any existing theory, the applicant believes that the hydroxyl groups of the polyol may have a similar structure to the silanol groups in the silane coupling agent, or that there may be some kind of hydrogen bond between them, thereby slowing down the polycondensation of the silane coupling agent.

[0044] In this application, the addition polymer containing two or more hydroxyl groups includes polyvinyl alcohol, partially hydrolyzed polyvinyl acetate, and homopolymers or copolymers of hydroxyethyl methacrylate and hydroxypropyl methacrylate.

[0045] In this application, the polyol is preferably triethanolamine.

[0046] In this application, the water-soluble thermosetting bio-based adhesive comprises 80wt%-20wt% of water-soluble bio-based raw material and 20wt%-80wt% of water-soluble bio-based raw material curing agent.

[0047] Preferably, the water-soluble bio-based raw material includes, but is not limited to, water-soluble sugars, water-soluble amino acids, water-soluble pregelatinized starch, or water-soluble modified lignin solution, wherein the water-soluble sugars include water-soluble corn syrup, water-soluble glucose, water-soluble sucrose, and fructose, etc.

[0048] Preferably, the water-soluble bio-based raw material curing agent includes, but is not limited to, one or more of polyamines, polyols, polycarboxylic acids, isocyanates, epoxy resins, or other curing agents that can react with bio-based raw materials.

[0049] In this application, one end of the compatible reactive silane coupling agent comprises a siloxane group, and the other end comprises a reactive functional organic group. The siloxane group is stable and compatible with the remaining components in the single-component formaldehyde-free setting agent at room temperature for a long period of time, and the reactive functional organic group can react with the formaldehyde-free adhesive at high temperature.

[0050] Preferably, the compatible reactive silane coupling agent includes epoxy siloxane monomolecular coupling agents (the epoxy siloxane monomolecular coupling agents described in this invention are essentially commonly used traditional epoxy siloxane coupling agents; to distinguish them from the "epoxy siloxane oligomer coupling agents" hereinafter referred to in this invention, this invention uniformly defines traditional epoxy siloxane coupling agents as epoxy siloxane monomolecular coupling agents, the same below) epoxy siloxane monomolecular coupling agents, epoxy siloxane oligomer coupling agents, amino silane coupling agents, and combinations thereof.

[0051] In this application, the epoxysiloxane monomolecular coupling agents include, but are not limited to, 3-(2,3-epoxypropoxy)propyltrimethoxysilane (KH560 in this application), 3-(2,3-epoxypropoxy)propyltriethoxysilane (KH561 in this application), 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane, 3-(2,3-epoxypropoxy)propylmethyldiethoxysilane (1872 in this application), 2-(3,4-epoxycyclohexane)ethyltrimethoxysilane (1873 in this application), and 2-(3,4-epoxycyclohexane)ethyltriethoxysilane (1874 in this application).

[0052] In this application, the epoxysiloxane oligomer coupling agent includes, but is not limited to, 3-epoxypropoxypropylalkoxysilane oligomer (designated 4721 in this application), particularly 3-epoxypropoxypropylalkoxysilane oligomer with a molecular weight of 500-2000.

[0053] In this application, the aminosilane coupling agent includes, but is not limited to, one or more of 3-aminopropyltrimethoxysilane (KH551 in this application), 3-aminopropyltriethoxysilane (KH550 in this application), 3-aminopropylmethyldiethoxysilane (KH552 in this application), N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (KH792 in this application) and N-(2-aminoethyl)-3-aminopropyldimethoxysilane (KH602 in this application).

[0054] Preferably, the compatible reactive silane coupling agent is selected from one or more of the codes KH550, KH560, KH561, 1872 and 4721 in this application; more preferably, it is selected from one or more of the codes 1872 and 4721 in this application; even more preferably, it is 4721 with a molecular weight of 500-2000.

[0055] The applicant has discovered that using 4721 with a molecular weight of 500-2000 as a compatible reactive silane coupling agent can extend the pot life of the single-component formaldehyde-free setting agent to more than 6 months.

[0056] In this application, the single-component formaldehyde-free hairspray may further include the following components in the following proportions:

[0057] 0-5 parts by weight of water-repellent agent;

[0058] Dust-proof oil: 0.1-10 parts by weight;

[0059] One part by weight is calculated based on 1 kg.

[0060] In this application, the hydrophobic agent is at least one of polydimethylsiloxane, modified hydroxyl polydimethylsiloxane, and modified hydrogen-based polydimethylsiloxane.

[0061] The applicant has discovered that when a hydrophobic agent is added to the single-component formaldehyde-free setting agent, the mineral wool products treated with the single-component formaldehyde-free setting agent are hydrophobic and moisture-proof, and their surfaces have a "lotus leaf" hydrophobic and moisture-proof effect, which can effectively prevent water molecules from adsorbing onto the glass fiber surface and improve the hydrophobic performance of the mineral wool.

[0062] In this application, preferably, the hydrophobic agent and the first emulsifier are premixed to form a hydrophobic emulsion, wherein the first emulsifier contains at least one first nonionic surfactant.

[0063] In this application, the first nonionic surfactant comprises a compound obtained by an addition condensation reaction of a fatty alcohol and ethylene oxide, optionally having the general formula [RO(C2H4O]. n [-H], where R represents a C6-C18 fatty alcohol group, n = 3-100, preferably 6-23.

[0064] More preferably, the first nonionic surfactant is selected from at least two of polyoxyethylene lauryl ether-3, polyoxyethylene lauryl ether-4, polyoxyethylene lauryl ether-7, polyoxyethylene lauryl ether-9, polyoxyethylene lauryl ether-15, polyoxyethylene lauryl ether-20, polyoxyethylene lauryl ether-23, polyoxyethylene C16-C18 alcohol ether-6, polyoxyethylene C16-C18 alcohol ether-12, and polyoxyethylene C16-C18 alcohol ether-20.

[0065] In this application, based on the total solid content of the single-component formaldehyde-free setting agent, the amount of the first nonionic surfactant is 0.1-5 parts by weight, preferably 0.5-3 parts by weight.

[0066] The applicant has discovered that excessive use of the first nonionic surfactant can lead to a decrease in the wet strength of mineral wool products treated with a single-component formaldehyde-free setting agent, while insufficient use can result in uneven and inadequate dispersion of the hydrophobic agent after it is added to the preparation system, thereby reducing the product stability of the single-component formaldehyde-free setting agent.

[0067] The applicant has discovered that, compared with commonly used anionic surfactants, the use of nonionic surfactants can minimize the damage to the wet strength of single-component formaldehyde-free setting agents while ensuring sufficient emulsification of the hydrophobic agent. This is not limited to any existing theory. The applicant believes that this is because the hydrophilic group of the first nonionic surfactant contains hydroxyl groups, which can react with the unsaturated carboxyl groups in the single-component formaldehyde-free setting agent, thereby maintaining a high wet strength in the single-component formaldehyde-free setting agent.

[0068] In this application, the dustproof oil is based on at least one of mineral base oil, self-emulsifying mineral oil, corn oil, and rapeseed oil. The mineral base oil may include, but is not limited to, one or more of 150SN, 200SN, 250SN, 325SN, 350SN, 500SN, or 650SN.

[0069] The applicant discovered that when the aforementioned dust-proof oil is added to the single-component formaldehyde-free setting agent, the mineral wool becomes more flexible after being treated with the single-component formaldehyde-free setting agent, making the mineral wool fibers less prone to breakage and dispersion during the cutting process, reducing dust generated during production and use, thereby reducing the hazards caused by dust to production and construction personnel.

[0070] In this application, preferably, the dust-proof oil is premixed with the second emulsifier to form an emulsion, the second emulsifier comprising at least one second nonionic surfactant, the second nonionic surfactant being selected from C12-C18 fatty acid glycerides, specifically including at least one of glyceryl laurate, glyceryl tetradecanoate, glyceryl hexadecanoate, and glyceryl stearate.

[0071] The applicant has discovered that using C12-C18 fatty acid glycerides as a second emulsifier minimizes the damage to the wet strength of the single-component formaldehyde-free setting agent while ensuring sufficient emulsification of the stabilized dust-proof oil. Therefore, this application preferably uses C12-C18 fatty acid glycerides as the second emulsifier.

[0072] In this application, based on the total solid content of the single-component formaldehyde-free setting agent, the amount of the second nonionic surfactant is 0.1-5 parts by weight, preferably 0.5-3 parts by weight.

[0073] The applicant has discovered that excessive use of the second nonionic surfactant can lead to a decrease in the wet strength of mineral wool products treated with a single-component formaldehyde-free setting agent, while insufficient use can result in uneven and inadequate dispersion of the dust-proof oil after it is added to the preparation system, thereby reducing the product quality of the single-component formaldehyde-free setting agent.

[0074] In this application, water may be added to the single-component formaldehyde-free hairspray as needed. The applicant has found that adding an appropriate amount of water to the single-component formaldehyde-free hairspray can reduce the viscosity of the single-component formaldehyde-free hairspray, making it easier to transport and use.

[0075] Preferably, the water is purified water, tap water, or other circulating water that does not affect the performance of the setting agent. Further, based on the solid content of the single-component formaldehyde-free setting agent being 100%, the amount of water added can be calculated as water weight: setting agent weight = (1-10):1.

[0076] Furthermore, defoamers, bactericides, dyes, and other functional additives can be added to this formula as needed.

[0077] In this application, the single-component formaldehyde-free hairspray comprises the following components:

[0078]

[0079] The pH of the fixative system is 3.0 to 5.0, with 1 kg as one part by weight.

[0080] The single-component formaldehyde-free setting agent provided by the present invention is a formaldehyde-free copolymer composition, wherein "formaldehyde-free" means that each component in the composition is basically free of formaldehyde, and that the curing process does not release formaldehyde, nor does it generate or release formaldehyde during the treatment of mineral wool.

[0081] Secondly, the present invention also provides a method for determining the pot life of a mineral wool fixative, the method comprising:

[0082] The mineral wool stabilizer to be tested was cured under high temperature conditions, and samples were taken sequentially according to the first time sequence.

[0083] The mineral wool stabilizer to be tested was cured at room temperature, and samples were taken sequentially according to the second time series.

[0084] The apparent properties, dry strength, and wet strength of each sample were tested sequentially.

[0085] In this application, the apparent properties include whether there is stratification, precipitation, or flocculation.

[0086] In this application, the dry strength test method for the single-component formaldehyde-free sizing agent can be performed with reference to Appendix C of the standard GB / T34181-2017 "Sizing Agent for Mineral Wool Insulation Products". When referring to the above standard, this application uses the solid content of the single-component formaldehyde-free sizing agent to replace the premixed phenolic resin in Appendix C, and changes the drying time from 180℃ / 20min to 180℃ / 30min. Other steps remain unchanged. The wet strength test conditions are 90% humidity and 40℃ for 24 hours before the bonding strength test.

[0087] In the bonding strength test described in this invention, the resin content is uniformly tested at 5% (by weight). In this application, the temperature condition can be an oven at 60±2℃, and the first time series can be 0 weeks, 3 weeks, 6 weeks, and 12 weeks.

[0088] In this application, the ambient temperature condition can be 25±2℃, and the second time series can be 0 months, 3 months, 6 months, and 12 months.

[0089] The applicant discovered that high-temperature testing accelerates chemical reactions by increasing temperature, which can quickly test the high-temperature resistance and stability of fixatives. This can be used for preliminary screening of fixatives, and then room-temperature testing can be performed on this basis, which can greatly save testing time.

[0090] The method includes the following steps:

[0091] Step 1: Curing the mineral wool fixative to be tested under high temperature conditions and taking samples sequentially according to the first time sequence;

[0092] Step 2: Cure the mineral wool fixative to be tested at room temperature and take samples sequentially according to the second time series;

[0093] Step 3: Test the apparent properties, dry strength, and wet strength of each sample one by one;

[0094] Step 4: If the test result of the mineral wool sizing agent meets any one of the following conditions, then the mineral wool sizing agent is considered invalid. The usable period of the mineral wool sizing agent is the time from the time the mineral wool sizing agent is prepared to the time it becomes invalid:

[0095] 1) Dry strength < 4.0 MPa;

[0096] 2) Wet strength < 3.0 MPa;

[0097] 3) The dry strength is less than 90% of that of freshly prepared sizing agents;

[0098] 4) The wet strength is less than 90% of that of the freshly prepared setting agent.

[0099] Furthermore, the single-component styling agent of the present invention, according to the above-mentioned pot life test method, has a pot life of at least >3 months at room temperature (20-25°C), that is, after being placed at room temperature for 3 months, its dry strength is >4.0 MPa and its wet strength is >3.0 MPa, and its dry strength is >90% and its wet strength is >90% of that of the freshly prepared styling agent; further still, the single-component styling agent with a preferred coupling agent has a pot life of >6 months at room temperature, that is, after being placed at room temperature for 6 months, its dry strength is >4.0 MPa and its wet strength is >3.0 MPa, and its dry strength is >90% and its wet strength is >90% of that of the freshly prepared styling agent; further still, with a preferred coupling agent and other conditions, the pot life at room temperature can be >12 months, with a dry strength >4.0 MPa and a wet strength >3.0 MPa, and its dry strength is >90% and its wet strength is >90% of that of the freshly prepared styling agent.

[0100] In existing technologies, in the mineral wool field, silane coupling agents, water-repellent agents, and dust-proofing oils are all prepared on-site, rather than pre-formulated as single-component formaldehyde-free sizing agents. For example, Feng Shaoyuan of Beijing Taier Chemical Co., Ltd., in his article "Research on Phenolic Resin System for Rock Wool Production" published at the 2014 Annual Meeting of the China Thermal Insulation and Energy Saving Materials Association on November 1, 2014, stated that "the method and timing of adding organosilane coupling agent KH550 during rock wool production has a significant impact on the entire phenolic resin system. Improper addition not only fails to utilize the coupling agent's function but also damages the effective components in the phenolic resin, causing adverse effects. Organosilane coupling agent KH550 hydrolyzes relatively quickly..." "KH550 should be added last to the rock wool phenolic resin system solution and used as soon as possible." Wang Xiaolei of Sinoma Science & Technology Co., Ltd., in his article "Research on Adhesive System for Rock Wool Production" published in "China Adhesives" (Vol.25 No.4, Apr.2016), systematically summarized the specific process of using adhesives in rock wool and proposed that "adhesive preparation methods can be divided into two types according to product requirements and production line specifications: ① pipeline mixing mode, that is, various raw materials are transported to pipeline mixers through pumps and solenoid valves for mixing and then used directly; ② tank mixing mode, that is, various raw materials are transported to mixing tanks through pumps and solenoid valves for stirring and mixing."

[0101] Compared with existing technologies, the single-component formaldehyde-free setting agent provided in this application avoids the use of formaldehyde at the source, so that no formaldehyde is released during the curing process, making it green and environmentally friendly. Furthermore, the single-component formaldehyde-free setting agent overcomes the technical prejudice inherited from the long-term use of phenolic resin setting agents. It is a pre-made, ready-to-use setting agent. During use, only water needs to be added as needed. No other additives need to be added to the setting agent, making it convenient to use, more suitable for continuous production, reducing labor costs and equipment investment costs, and facilitating the quality control of the setting agent.

[0102] The technological bias in this industry stems from the following aspects:

[0103] 1) For a long time, due to the short pot life caused by the addition of urea, ammonium sulfate and other additives to phenolic resin, the phenolic resin fixative must be prepared on the spot. Therefore, after switching to formaldehyde-free resin, the process of preparing on the spot is still the same as that of phenolic resin.

[0104] 2) Coupling agents are essential additives for the preparation of mineral wool sizing agents. However, coupling agents are usually unstable in aqueous systems, which affects the performance of the sizing agent and further limits the attempt to prepare ready-to-use one-component formaldehyde-free sizing agents.

[0105] 3) In the composition of mineral wool products, based on the total weight of the mineral wool products, the weight ratio of the sizing agent is generally only 1.5wt%-10wt%, and the rest is mineral wool fiber. Therefore, for mineral wool products, the quality of mineral wool fiber is more important than the quality of the sizing agent. However, in the quality testing of mineral wool products, it is impossible to separate the sizing agent and mineral wool fiber for separate quality evaluation. Moreover, the quality of mineral wool fiber fluctuates greatly with production batches, that is, the quality stability of mineral wool fiber is poor. This means that it is impossible to accurately estimate the quality of the sizing agent by only evaluating the quality of mineral wool products, which further increases the testing costs in the mineral wool industry.

[0106] 4) The mineral wool industry is a continuous large-scale production industry, with each production line typically producing up to 20,000 tons per year. Currently, there are no relevant small-scale or pilot-scale mineral wool production lines in China. Each test must be conducted directly on a large-scale production line, increasing testing and switching costs. Detailed Implementation

[0107] Exemplary embodiments will now be described in detail. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of methods consistent with some aspects of the invention as detailed in the appended claims.

[0108] (I) Experimental Methods

[0109] After the single-component formaldehyde-free setting agent was prepared, multiple samples were taken to test its solid content, dry bond strength, wet bond strength, stability at room temperature, and high-temperature accelerated stability.

[0110] The standards and specifications referenced for each test item are as follows:

[0111] (1) The test method for solid content shall be performed in accordance with GB / T 34181-2017, and the test conditions shall be 120 degrees / 2h.

[0112] (2) The test methods for bonding strength and formaldehyde content shall be carried out in accordance with the standard GB / T 34181-2017 "Styling Agent for Mineral Wool Insulation Products". In the dry bonding strength test, the resin content shall be uniformly tested at 5%. The curing conditions for wet bonding strength are 90% humidity and 40℃ for 24 hours.

[0113] (3) Place it in a normal temperature environment and observe the apparent properties of the fixative at 0 months, 3 months, 6 months and 12 months respectively, and observe whether there are any deterioration phenomena such as layering, precipitation or flocculation.

[0114] If the applicable period ends before the observation period expires during the testing process, the subsequent testing will be stopped based on the principles of saving resources and improving efficiency.

[0115] (4) Place it in a high temperature environment and observe the apparent properties of the fixative at 0, 3, 6 and 12 weeks respectively, and observe whether there are any deterioration phenomena such as layering, precipitation or flocculation.

[0116] If the applicable period ends before the observation period expires during the testing process, the subsequent testing will be stopped based on the principles of saving resources and improving efficiency.

[0117] (5) For the testing methods of mineral wool properties, refer to the following standards:

[0118] GB / T 13350-2017 Glass wool and its products for thermal insulation

[0119] GB / T 19686-2015 Rock Wool Insulation Products for Buildings

[0120] GB / T 11835-2016 Rock wool, slag wool and their products for thermal insulation

[0121] In the following examples and comparative examples, the formaldehyde content of the mineral wool was tested in accordance with the method for formaldehyde-free glass wool specified in GB / T 13350-2017.

[0122] (ii) Unless otherwise specified, all parts in the following embodiments refer to parts by weight, and the number of parts is calculated based on 100% solid content.

[0123] For ease of explanation, the following discussion addresses the factors affecting the performance of single-component formaldehyde-free hairspray:

[0124] 1. The effect of coupling agents on the performance of single-component formaldehyde-free hairspray.

[0125] Example

[0126] Examples 1-8

[0127] Examples 1-8 were prepared using the same method and with essentially the same components, differing only in the coupling agent used. Specifically, the components used to prepare the single-component formaldehyde-free setting agent were formulated in the following proportions:

[0128]

[0129]

[0130] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 3.2.

[0131] The coupling agents used in Examples 1-8 are specifically shown in Table 1-1 below:

[0132] Table 1-1 Coupling agents used in Examples 1-8

[0133] Example Coupling agent Example 1 Coupling agent KH560 Example 2 Coupling agent KH561 Example 3 Coupling agent 1872 Example 4 Coupling agent 1873 Example 5 Coupling agent 1874 Example 6 Coupling agent 4721 Example 7 Coupling agent KH550 Example 8 Coupling agent KH792

[0134] Among them, coupling agent 4721 is a 3-epoxypropoxypropylalkoxysilane oligomer coupling agent from Evonik Specialty Chemicals Ltd., M n It is 800-1200.

[0135] Comparative Example

[0136] Comparative Example 1

[0137] A single-component formaldehyde-free hairspray was prepared according to the following component ratio:

[0138]

[0139] The phenolic resin Prefere 72-5563 was purchased from Prefere 72-5563 for glass wool produced by Taier Chemical (Nanjing) Co., Ltd.

[0140] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 7.5.

[0141] It is evident that the system prepared in this comparative example is weakly alkaline.

[0142] Comparative Examples 2-3

[0143] Comparative Examples 2 and 3 were prepared using the same methods and had essentially the same components as Example 1, differing only in the coupling agents used. Specifically, the coupling agents used in Comparative Examples 2 and 3 are shown in Table 1-2 below:

[0144] Table 1-2 Coupling agents used in Comparative Examples 2-3

[0145] Comparative Example Coupling agent Comparative Example 2 Vinyltris(2-methoxyethoxy)silane (KH172) Comparative Example 3 none

[0146] 1.1 The apparent stability of the products obtained in Examples 1-8 and Comparative Examples 1-3 was tested according to the aforementioned method. The test results are shown in Tables 1-3 below:

[0147] Table 1-3 Results of apparent stability tests on the products obtained in Examples 1-8 and Comparative Examples 1-3

[0148]

[0149] Based on the above apparent performance test results, no obvious abnormalities were observed in the single-component formaldehyde-free setting agent formulations of Examples 1-8 with added silane epoxy and amino series coupling agents, which is basically consistent with the scheme of Comparative Example 3 without added coupling agent.

[0150] In addition, Comparative Example 1, which uses phenolic resin as the matrix component, showed apparent stability of no more than one week under high temperature conditions.

[0151] 1.2 The dry strength stability of the products obtained in Examples 1-8 and Comparative Examples 1-3 were tested according to the aforementioned method. The test results are shown in Tables 1-4 below:

[0152] Table 1-4 Results of dry strength stability tests on the products obtained in Examples 1-8 and Comparative Examples 1-3

[0153]

[0154] 1.3 The wet strength stability of the products obtained in Examples 1-8 and Comparative Examples 1-3 were tested according to the aforementioned method. The test results are shown in Tables 1-5 below:

[0155] Table 1-5 Results of wet strength stability tests on the products obtained in Examples 1-8 and Comparative Examples 1-3

[0156]

[0157]

[0158] As can be seen from the results in Tables 1-1 to 1-5 above, when the amount of coupling agent added is 0.2 parts and the pH value of the setting agent system is 3.2, the setting agents prepared in all the above examples have a room temperature pot life of >3 months, dry strength >4.0 MPa, wet strength >3.0 MPa, and the dry strength is >90% of that of the freshly prepared setting agent, and the wet strength is >90% of that of the freshly prepared setting agent; among them, the setting agents with added coupling agents KH560, 1872 and KH550, For setting agents with a room temperature service life > 6 months, dry strength > 4.0 MPa, and wet strength > 3.0 MPa, with dry strength > 90% and wet strength > 90% of the freshly prepared setting agent; for setting agents with coupling agents KH561, 4721, and KH792, the room temperature service life > 12 months, dry strength > 4.0 MPa, and wet strength > 3.0 MPa, with dry strength > 90% and wet strength > 90% of the freshly prepared setting agent.

[0159] 2. Effects of pH and polyols on the pot life of the setting agent system

[0160] Example

[0161] Examples 9-11

[0162] The formulations of Examples 9-11 are the same as those of Example 2, except that hydrochloric acid is used to adjust the pH of the product system after mixing.

[0163] The formulations of Comparative Examples 4 and 5 are the same as those of Example 2, except that ammonia was used to adjust the pH of the product system after mixing. The formulation of Comparative Example 6 is similar to that of Example 2, except that 100 parts by weight of polyacrylic acid resin polymer were used, the raw materials did not include polyols (i.e., triethanolamine), and ammonia was used to adjust the pH of the product system after mixing.

[0164] The final pH values ​​of the product systems in each embodiment and comparative example are shown in Table 2-1 below:

[0165] Table 2-1 Final pH of the systems in Examples 9-11 and Comparative Examples 4-6

[0166] Example Final pH of the setting agent system Example 9 0.5 Example 10 2.2 Example 11 5.0 Comparative Example 4 8.0 Comparative Example 5 10.5 Comparative Example 6 5.0

[0167] 2.1 The apparent stability of the products obtained in Examples 9-11 and Comparative Examples 4-6 was tested according to the aforementioned method. The test results are shown in Table 2-2 below:

[0168] Table 2-2 Results of apparent stability tests on the products obtained in Examples 9-11 and Comparative Examples 4-6

[0169]

[0170] As can be seen from the results in Table 2-2 above, the pH value of the setting agent system has the best stability and the longest pot life in the range of 3.0-5.0. Under alkaline conditions, the coupling agent will have stability problems such as precipitation as the time at high temperature or room temperature is prolonged, with only 3 months of pot life at room temperature, or even less. At the same time, the stability test results of Comparative Example 6 and Example 11 show that the stability of the setting agent without the addition of polyol is not as good as that of Example 11 with the addition of polyol. Therefore, the polyol in the formula can play a role in improving stability and extending the pot life of the setting agent.

[0171] Therefore, the pH value of the setting agent in this invention is most preferably between 3.0 and 5.0.

[0172] 3. Pot life test for different coupling agent contents

[0173] Examples 12-17

[0174] Examples 12-17 were prepared using the same methods and formulas as Example 1, differing only in the type and amount of coupling agent used. The specific types and amounts of coupling agents used in Examples 12-17 are shown in Table 3-1 below.

[0175] Table 3-1 Coupling agents and dosages used in Examples 12-17

[0176] Example Coupling agent Coupling agent dosage / parts by weight Example 12 Coupling agent KH561 0.5 Example 13 Coupling agent KH561 0.8 Example 14 Coupling agent 4721 0.5 Example 15 Coupling agent 4721 0.8 Example 16 Coupling agent KH792 0.5 Example 17 Coupling agent KH792 0.8 Comparative Example 7 Coupling agent KH561 1.5 Comparative Example 8 Coupling agent 4721 1.5 Comparative Example 9 Coupling agent KH792 1.5

[0177] 3.1 The apparent stability of the products obtained in Examples 12-17 and Comparative Examples 7-9 were tested according to the aforementioned method. The test results are shown in Table 3-2 below:

[0178] Table 3-2 Results of apparent stability tests on the products obtained in Examples 12-17 and Comparative Examples 7-9

[0179]

[0180]

[0181] 3.2 The dry strength stability tests were performed on the products obtained in Examples 12-17 and Comparative Examples 7-9 according to the aforementioned method. The test results are shown in Table 3-3 below:

[0182] Table 3-3 Results of dry strength stability tests on the products obtained in Examples 12-17 and Comparative Examples 7-9

[0183]

[0184] 3.3 The wet strength stability of the products obtained in Examples 12-17 and Comparative Examples 7-9 were tested according to the aforementioned method. The test results are shown in Table 3-4 below:

[0185] Table 3-4 Results of wet strength stability tests on the products obtained in Examples 12-17 and Comparative Examples 7-9

[0186]

[0187]

[0188] As can be seen from the results in Tables 3-1 to 3-4 above, the stability and dry-wet strength of the setting agent are optimal when the amount of coupling agent added is 0.2-0.8 parts by weight. The applicable period at room temperature can reach 12 months. If the amount of coupling agent added is further increased, not only will the dry-wet strength of the setting agent not increase, but precipitation may also occur in the setting agent system due to the excessive amount of coupling agent, affecting the stability of the setting agent and increasing the cost of the setting agent. In summary, the optimal amount of coupling agent is 0.2-0.5 parts.

[0189] 4. Pot life test of different formulations of setting agent + coupling agent + water repellent + dust-proof oil

[0190] Example 18

[0191]

[0192] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 7.5.

[0193] In this embodiment, the base oil and polydimethylsiloxane were pre-emulsified into a stable aqueous emulsion using a high-speed disperser at a speed of 500-3000 rpm.

[0194] Example 19

[0195]

[0196] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 3.3.

[0197] In this embodiment, the composition and preparation method of the bio-based adhesive can be found in Example 8 of CN102363721A; the corn oil and modified hydroxyl polydimethylsiloxane are pre-emulsified into a stable aqueous emulsion using a high-speed disperser at a speed of 500-3000 rpm.

[0198] Example 20

[0199] 100 parts of bio-based adhesive, the composition of which is consistent with Example 8 of CN102363721A.

[0200] Coupling agent KH792 0.5 parts

[0201]

[0202] Wherein, based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 3.3.

[0203] In this embodiment, the composition and preparation method of the bio-based adhesive can be found in Example 8 of CN102363721A; the emulsifiable mineral oil and the modified hydrogen-based polydimethylsiloxane are pre-emulsified into a stable aqueous emulsion using a high-speed disperser at a speed of 500-3000 rpm.

[0204] Comparative Example 10

[0205] The preparation method and formulation of this comparative example are the same as those of Example 18, with the only difference being that the anionic surfactant sodium dodecylbenzenesulfonate is used instead of the nonionic surfactant polyoxyethylene lauryl ether-20 in the base oil 350SN. The specific formulation is as follows:

[0206]

[0207] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 7.5.

[0208] In this comparative example, the base oil 350SN and the polydimethylsiloxane were pre-emulsified into a stable aqueous emulsion using a high-speed disperser at a speed of 500-3000 rpm.

[0209] Comparative Example 11

[0210] The preparation method and formulation of this comparative example are the same as those of Example 18, with the only difference being that the surfactant used in the dust-proof oil is the anionic surfactant sodium dodecylbenzenesulfonate. The specific formulation is as follows:

[0211]

[0212]

[0213] Based on the total weight of the setting agent system, the solid content of the setting agent system is 50%, and the pH value of the setting agent system is 7.5.

[0214] In this comparative example, the base oil and polydimethylsiloxane were pre-emulsified into a stable aqueous emulsion using a high-speed disperser at a speed of 500-3000 rpm.

[0215] 4.1 The apparent stability of the products obtained in Examples 18-20 and Comparative Examples 10-11 was tested according to the aforementioned method. The test results are shown in Table 4-1 below:

[0216] Table 4-1 Apparent stability test results of the products obtained in Examples 18-20 and Comparative Examples 10-11

[0217]

[0218] 4.2 The dry strength stability tests were conducted on the products obtained in Examples 18-20 and Comparative Examples 10-11 according to the aforementioned method. The test results are shown in Table 4-2 below:

[0219] Table 4-2 Results of dry strength stability tests on the products obtained in Examples 18-20 and Comparative Examples 10-11

[0220]

[0221] 4.3 The wet strength stability tests were conducted on the products obtained in Examples 18-20 and Comparative Examples 10-11 according to the aforementioned method. The test results are shown in Tables 1-5 below:

[0222] Table 4-3 Results of wet strength stability tests on the products obtained in Examples 18-20 and Comparative Examples 10-11

[0223]

[0224]

[0225] As can be seen from the results in Tables 4-1 to 4-3 above, the further addition of water-repellent agents and dust-proof oils to the setting agent formulation did not significantly damage the stability of the setting agent product. Although the dry strength and wet strength may decrease due to the addition of dust-proof oils, they still meet the requirements for the pot life. The products in the above examples still have a 12-month pot life at room temperature. However, after using anionic surfactants in Comparative Examples 10-11, the wet strength of the setting agent was significantly reduced. Therefore, this application does not recommend the use of anionic surfactants.

[0226] Test case

[0227] The experimental examples in this application used the setting agent prepared in the embodiments of this application to prepare mineral wool after curing for a specific period of time, as shown in Table 5-1 below:

[0228] Table 5-1 Test Parameters for Experimental Examples

[0229]

[0230] The above-mentioned test samples were tested according to the method in (I), and the results are shown in Table 5-2 below:

[0231] Table 5-2 Comparison of basic performance between Test Example 1 and Test Example 2

[0232] Serial Number Basic performance GB / T 19686-2015 requirements Experimental Example 1 Experimental Example 2 1 Thickness (mm) Meets national standards Meets national standards Meets national standards 2 <![CDATA[Unit weight (kg / m 3 )]]> Meets national standards Meets national standards Meets national standards 3 Moisture absorption rate (%) ≤0.5％ 0.4 0.3 4 Organic matter content (%) As needed 4％ 4％ 5 Hydrophobicity (%) ≥98.0 ≥99.2 ≥98.6 6 Fiber diameter (µm) ≤6.0 5.8 5.9 7 Combustion performance Grade A Grade A Grade A 8 <![CDATA[Formaldehyde content (mg / m 3 )]]> Not detectable Not detected Not detected

[0233] Table 5-3 Comparison of basic performance between Test Example 3 and Test Example 4

[0234] Serial Number Basic performance GB / T13350-2017 requirements Experimental Example 3 Test Example 4 1 Thickness (mm) Meets national standards Meets national standards Meets national standards 2 <![CDATA[Unit weight (kg / m 3 )]]> Meets national standards Meets national standards Meets national standards 3 Moisture absorption rate (%) ≤1.0 0.3 0.3 4 Organic matter content (%) As needed 3％ 3％ 5 Hydrophobicity (%) ≥98.0 98.6 ≥98.4 6 Fiber diameter (µm) ≤7.0 6.6 6.8 7 Combustion performance Grade A Grade A Grade A 8 <![CDATA[Formaldehyde content (mg / m 3 )]]> Not detectable Not detected Not detected

[0235] Table 5-4 Comparison of basic performance between Test Example 5 and Test Example 6

[0236] Serial Number Basic performance GB / T 11835-2016 requirements Experimental Example 5 Experimental Example 6 1 Thickness (mm) Meets national standards Meets national standards Meets national standards 2 <![CDATA[Unit weight (kg / m 3 )]]> Meets national standards Meets national standards Meets national standards 3 Moisture absorption rate (%) ≤1.0 0.4 0.4 4 Organic matter content (%) ≤4.0 2.8％ 2.8％ 5 Hydrophobicity (%) ≥98.0 ≥99.8 ≥99.7 6 Fiber diameter (µm) ≤6.0 6.2 6.4 7 Combustion performance Grade A Grade A Grade A 8 <![CDATA[Formaldehyde content (mg / m 3 )]]> Not detectable Not detected Not detected

[0237] As can be seen from the results shown in Tables 5-2 to 5-4 above, the single-component setting agent prepared in the embodiments of this application still has essentially the same properties as the newly prepared setting agent after 12 months of curing at room temperature.

[0238] The present application has been described in detail above with reference to specific embodiments and exemplary examples; however, these descriptions should not be construed as limiting the present application. Those skilled in the art will understand that various equivalent substitutions, modifications, or improvements can be made to the technical solutions and implementation methods of the present application without departing from the spirit and scope of the present application, and all such modifications and improvements fall within the scope of the present application. The scope of protection of the present application is determined by the appended claims.

Claims

1. A single-component, formaldehyde-free setting agent specifically for mineral wool, characterized in that, Based on 100% solid content, the single-component formaldehyde-free setting agent comprises the following components in the indicated weight ratios: 100 parts by weight of formaldehyde-free adhesive; 0.1-0.8 parts by weight of a compatible reactive silane coupling agent; One part by weight is calculated based on 1 kg. The formaldehyde-free adhesive is a non-trialdehyde resin that does not use formaldehyde as a direct raw material; including a water-soluble thermosetting polyacrylate formaldehyde-free adhesive; the water-soluble thermosetting polyacrylate includes 60wt%-90wt% of unsaturated carboxylic acid oligomers and 10wt%-40wt% of polyols. The compatible reactive silane coupling agents include epoxy siloxane monomolecule coupling agents, epoxy siloxane oligomer coupling agents, amino silane coupling agents, and combinations thereof. The pH of the single-component formaldehyde-free setting agent is 3.0~5.0; The single-component formaldehyde-free setting agent has a room temperature service life of more than 6 months.

2. The single-component formaldehyde-free setting agent according to claim 1, characterized in that, The epoxysiloxane monomolecule coupling agent comprises one or more of the following: 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 3-(2,3-epoxypropoxy)propyltriethoxysilane, 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane, 3-(2,3-epoxypropoxy)propylmethyldiethoxysilane, 2-(3,4-epoxycyclohexane)ethyltrimethoxysilane, and 2-(3,4-epoxycyclohexane)ethyltriethoxysilane; and / or The epoxysiloxane oligomer coupling agent is a 3-epoxypropoxypropylalkoxysilane oligomer with a molecular weight of 500-2000; and / or The aminosilane coupling agent includes, but is not limited to, one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropylmethyldiethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, and N-(2-aminoethyl)-3-aminopropyldimethoxysilane.

3. The single-component formaldehyde-free setting agent according to claim 1, characterized in that, The coupling agent is selected from one or more of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 3-(2,3-epoxypropoxy)propyltriethoxysilane, 3-(2,3-epoxypropoxy)propylmethyldimethoxysilane, 3-(2,3-epoxypropoxy)propylmethyldiethoxysilane, 2-(3,4-epoxycyclohexane)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexane)ethyltriethoxysilane, 3-epoxypropoxypropylalkoxysilane oligomer, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropylmethyldiethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, and N-(2-aminoethyl)-3-aminopropyldimethoxysilane.

4. A method for determining the pot life of the single-component formaldehyde-free hairspray according to any one of claims 1-3, characterized in that, The method includes the following steps: Step 1: Curing the single-component formaldehyde-free hairspray to be tested at 60±2°C, and taking samples sequentially according to the first time series; the first time series is 0 weeks, 3 weeks, 6 weeks and 12 weeks; Step 2: Curing the single-component formaldehyde-free hairspray to be tested at room temperature, and taking samples sequentially according to the second time series; the second time series is 0 months, 3 months, 6 months and 12 months; Step 3: Test the apparent properties, dry strength, and wet strength of each sample one by one; Step 4: If the test result of the single-component formaldehyde-free hairspray meets any one of the following conditions, then the single-component formaldehyde-free hairspray is invalid. The usable period of the single-component formaldehyde-free hairspray is the time from the completion of preparation to its invalidation: 1) Dry strength < 4.0 MPa; 2) Wet strength < 3.0 MPa.

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