Two-component polyurethane sealant, method for preparing the same and use thereof
By designing a two-component polyurethane sealant, and through the reaction of a self-synthesized curing agent with a polyol component, adjusting the molecular weight and adding a cross-linking structure, the problems of existing polyurethane sealants requiring a primer and having low strength are solved, achieving high bonding strength and durability.
Patent Information
- Application Number
- CN202310077451.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-01-13
- Publication Date
- 2025-11-25
- Estimated Expiration
- 2043-01-13
AI Technical Summary
Existing polyurethane sealants require a primer to ensure good adhesion when bonding with glass, and their strength is not high.
A two-component polyurethane sealant is used. Component A includes polyether polyol, filler and first additive, while component B includes curing agent, thickener and second additive. The curing agent is synthesized in-house and reacts with the corresponding polyol component to adjust the molecular weight of the final reaction product. An appropriate amount of polyol is added to prepare a cross-linked structure to enhance the bonding strength.
This method achieves an interfacial adhesion force between the sealant and glass that is greater than the cohesive force, thereby improving the bond strength, enhancing the water-UV treatment performance, and increasing the sealant's durability and sealing properties.
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Figure BDA0004067298830000231
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of adhesive materials, in particular to a two-component polyurethane sealant and a preparation method and application thereof. BACKGROUND
[0002] Sealant is a material used to fill gaps (holes, joints, etc.). Elastic sealant is a product that combines bonding and sealing functions. The sealant for double-layer hollow glass is a special product used in the construction field. Double-layer hollow glass is a window glass product sealed around the edges with dry air or vacuum in the middle, which has excellent heat insulation performance and is mainly used for door and window glass. In the double-sealing hollow glass production process, the first sealing uses butyl rubber, and the second sealing uses polysulfide (PS), silicone (SR) or polyurethane (PU) elastic sealant. However, most of the polyurethane sealants currently used on the market need to be primed to ensure good adhesion to glass, and the strength is not high. SUMMARY
[0003] Therefore, it is necessary to provide a two-component polyurethane sealant and a preparation method thereof, which has high bonding strength and stable performance.
[0004] The first aspect of the present application provides a two-component polyurethane sealant, comprising component A and component B, wherein the component A comprises the following raw materials in mass percentage:
[0005] polyether polyol, 10% to 40%;
[0006] filler, 50% to 70%;
[0007] first additive, 0.01% to 32.2%;
[0008] The component B comprises the following raw materials in mass percentage:
[0009] curing agent, 60% to 85%;
[0010] thickening agent, 1% to 5%;
[0011] second additive, 11% to 38.5%;
[0012] The curing agent in the component B comprises the following raw materials in mass percentage:
[0013] isocyanate, 70% to 90%;
[0014] polyether polyol, 8% to 25%;
[0015] polyester polyol, 0.5% to 4%;
[0016] Third adjuvant, 0-4%;
[0017] The mass ratio of component A to component B is (10-18):1.
[0018] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:
[0019] (1) Based on the total mass of component A, the first auxiliary agent comprises the following raw materials by mass percentage:
[0020] Plasticizer, 0–30%; primary catalyst, 0.01%–0.2%; primary coupling agent, 0–2%.
[0021] (2) Based on the total mass of component B, the second auxiliary agent comprises the following raw materials by mass percentage:
[0022] Color paste, 10%–28%; second coupling agent, 1%–5%; first catalyst, 0–0.5%; plasticizer, 0–5%.
[0023] (3) Based on the total mass of the curing agent in component B, the third auxiliary agent comprises the following raw materials by mass percentage:
[0024] Chain extender, 0–3%; secondary catalyst, 0–1%.
[0025] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:
[0026] (1) The polyether polyols in component A include polyoxypropylene diol and / or polyoxypropylene triol.
[0027] Optionally, the molecular weight of the polyoxypropylene glycol is one or more of 1000, 2000, 4000 and 8000.
[0028] Optionally, the molecular weight of the polyoxypropylene triol is one or more of 300, 400, 500, 700 and 1000.
[0029] (2) The filler includes one or more of nano calcium carbonate, heavy calcium carbonate, activated heavy calcium carbonate, talc and light calcium carbonate.
[0030] (3) The polyether polyol in the curing agent of component B includes polyoxypropylene glycol.
[0031] Optionally, the molecular weight of the polyoxypropylene glycol is one or more of 1000, 2000, 4000 and 8000.
[0032] (4) The polyester polyol in the curing agent of component B includes phthalic anhydride polyester diol.
[0033] Optionally, the phthalic anhydride polyester diol has a molecular weight of one or more of 280, 350, 450 and 560.
[0034] (5) The isocyanate in the curing agent of component B includes one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate.
[0035] (6) The thickener of component B includes fumed silica.
[0036] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:
[0037] (1) The plasticizer includes one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate and dioctyl phthalate.
[0038] (2) The first catalyst includes one or more of tertiary amine catalysts and organometallic catalysts.
[0039] Optionally, the tertiary amine catalyst includes one or more of aliphatic amine catalysts, ester cyclic amine catalysts, and aromatic amine catalysts.
[0040] Optionally, the organometallic catalyst includes one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc-bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate.
[0041] (3) The first coupling agent includes one or more of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-aminopropyltriethoxysilane, bis-(γ-trimethoxysilylpropyl)amine and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane.
[0042] Optionally, the first coupling agent includes one or more of KH-560, KH-550, Momentive A-1170, and KH-792.
[0043] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:
[0044] (1) The color paste includes one or more of Calorie HC460, Calorie HC585 and Calorie HS461.
[0045] (2) The second coupling agent includes γ-(2,3-epoxypropoxy)propyltrimethoxysilane.
[0046] Optionally, the second coupling agent includes KH-560.
[0047] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:
[0048] (1) The chain extender includes one or more of 1,4-butanediol, ethylene glycol, diethylene glycol and 1,6-hexanediol.
[0049] (2) The second catalyst includes one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc bismuth composite catalyst, bismuth isooctanoate and zinc neodecanoate.
[0050] A second aspect of this application provides a method for preparing the two-component polyurethane sealant described in the first aspect of this application, comprising:
[0051] The components contained in component A are mixed and then subjected to heat treatment and dehydration treatment to obtain component A;
[0052] The curing agent is obtained by reacting a dehydrated polyether polyol with an isocyanate, followed by adding a dehydrated polyester polyol and reacting again.
[0053] The components contained in component B are mixed to obtain component B;
[0054] The two-component polyurethane sealant is obtained by mixing component A and component B at a mass ratio of (10-18):1 and then curing.
[0055] In some embodiments of this application, the step of mixing the components contained in component A and then subjecting them to heat treatment and dehydration includes:
[0056] The polyether polyol and the filler are mixed and heated to 80°C to 120°C, and dehydrated under vacuum for 1 to 5 hours until the water content drops below 600 ppm to obtain a premix; optionally, a plasticizer is added during the mixing process of the polyether polyol and the filler.
[0057] The premix is cooled to below 40°C, and a first catalyst is added. The mixture is stirred evenly under vacuum conditions. Optionally, a first coupling agent is also added during the mixing process of the premix and the first catalyst.
[0058] In some embodiments of this application, the preparation process of the curing agent in component B includes:
[0059] The dehydrated polyether polyol is reacted with isocyanate at a temperature of 70°C to 85°C for 0.5 h to 3 h under a nitrogen protective atmosphere. Optionally, the dehydrated polyether polyol is also mixed with a second catalyst.
[0060] Then, add dehydrated polyester polyol to react at a temperature of 70℃~85℃ for 0.5h~2h under a nitrogen protective atmosphere.
[0061] Optionally, after the dehydration-treated polyester polyol is added and reacted, a dehydration-treated chain extender is added to continue the reaction. The reaction temperature is 70℃~85℃, the reaction time is 0.5h~2h, and the reaction atmosphere is a nitrogen protective atmosphere.
[0062] In some embodiments of this application, the mixing process of the components contained in component B includes:
[0063] After the curing agent and color paste are mixed evenly under vacuum conditions, the second coupling agent is added and mixed evenly. The thickener is then added while stirring until the viscosity reaches (3 × 10⁻⁶). 4 ) mPa·s~(12×10 4 )mPa·s.
[0064] Optionally, the first catalyst and / or plasticizer may also be added during the step of adding the second coupling agent.
[0065] In some embodiments of this application, the method satisfies at least one of the following conditions:
[0066] (1) The vacuum degree of the vacuum condition is above 0.09 MPa;
[0067] (2) The stirring rate of the stirring is 50 r / min to 500 r / min.
[0068] The third aspect of this application provides an application of a two-component polyurethane sealant in insulating glass, the two-component polyurethane sealant including the two-component polyurethane sealant described in the first aspect of this application or a two-component polyurethane sealant prepared according to the method described in the second aspect of this application.
[0069] This application has the following beneficial effects:
[0070] The two-component polyurethane sealant provided in this application adjusts the molecular weight of the final reaction product by reacting a self-synthesized curing agent with the corresponding polyol component, and controls the molecular weight of the final reaction product within a specific and suitable range, so that the interfacial adhesion between the sealant and the glass is greater than the cohesive force of the sealant. Detailed Implementation
[0071] To facilitate understanding of this application, a more complete description will be provided below. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of this application.
[0072] For simplicity, this application only explicitly discloses some numerical ranges. However, any lower limit can be combined with any upper limit to form a range not explicitly stated; and any lower limit can be combined with other lower limits to form a range not explicitly stated, just as any upper limit can be combined with any other upper limit to form a range not explicitly stated. Furthermore, although not explicitly stated, every point or individual value between the endpoints of the range is included within that range. Therefore, each point or individual value can be used as its own lower or upper limit and combined with any other point or individual value or with other lower or upper limits to form a range not explicitly stated.
[0073] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the specification of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. It should be noted that, unless otherwise stated, the term "and / or" as used herein includes any and all combinations of one or more of the associated listed items, "above," "below," includes the stated number, and "one or more" with "multiple" means two or more.
[0074] The foregoing description of this application is not intended to describe every disclosed implementation or method. Instead, the following description provides more specific examples of exemplary embodiments. Throughout the application, guidance is provided through a series of embodiments that can be used in various combinations. The examples listed are representative only and should not be construed as exhaustive.
[0075] The first aspect of this application provides a two-component polyurethane sealant, comprising component A and component B, wherein component A comprises the following raw materials by mass percentage: polyether polyol, 10%–40%; filler, 50%–70%; and a first auxiliary agent, 0.01%–32.2%; component B comprises the following raw materials by mass percentage: curing agent, 60%–85%; thickener, 1%–5%; and a second auxiliary agent, 11%–38.5%; the curing agent in component B comprises the following raw materials by mass percentage: isocyanate, 70%–90%; polyether polyol, 8%–25%; polyester polyol, 0.5%–4%; and a third auxiliary agent, 0%–4%; the mass ratio of component A to component B is (10–18):1.
[0076] The two-component polyurethane sealant provided in this application, through the reaction of a self-synthesized curing agent with a corresponding polyol component, adjusts the molecular weight of the final reaction product and controls it within a specific suitable range, achieving an interfacial adhesion strength between the sealant and glass greater than the sealant's cohesive strength. Simultaneously, this application prepares a sealant with a cross-linked structure by adding an appropriate amount of polyol, improving the sealant's bonding strength, water-UV treatment performance, durability, and sealing properties.
[0077] In some embodiments, the first additive in component A comprises the following raw materials by mass percentage: plasticizer, 0-30%; first catalyst, 0.01%-0.2%; and first coupling agent, 0-2%.
[0078] In some embodiments, the second additive in component B comprises the following raw materials by mass percentage: color paste, 10% to 28%; second coupling agent, 1% to 5%; first catalyst, 0% to 0.5%; plasticizer, 0% to 5%.
[0079] In some embodiments, the third auxiliary agent in the B component curing agent comprises the following raw materials by mass percentage: chain extender, 0-3%; second catalyst, 0-1%.
[0080] In some embodiments, the first coupling agent comprises one or more of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-aminopropyltriethoxysilane, bis-(γ-trimethoxysilylpropyl)amine, and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane. Optionally, the first coupling agent comprises one or more of KH-560, KH-550, Momentive A-1170, and KH-792.
[0081] In some embodiments, the second coupling agent comprises γ-(2,3-epoxypropoxy)propyltrimethoxysilane. Optionally, the second coupling agent comprises KH-560.
[0082] In this application, after adding an appropriate coupling agent to components A and B, the coupling agent can interact with both the hydroxyl groups in inorganic materials and the long molecular chains in organic polymers, thereby coupling the two materials with different properties together. This enhances the interfacial interaction between the two-component polyurethane sealant and the glass, further increasing the adhesion between the two-component polyurethane sealant and the glass interface, and thus enabling cohesive failure.
[0083] In some embodiments, the polyether polyol in component A includes polypropylene glycol and / or polypropylene triol; optionally, the molecular weight of the polypropylene glycol is one or more of 1000, 2000, 4000 and 8000; optionally, the molecular weight of the polypropylene triol is one or more of 300, 400, 500, 700 and 1000.
[0084] In some embodiments, the type of filler is not particularly limited and can be selected according to actual needs. For example, the filler may include one or more of nano-calcium carbonate, heavy calcium carbonate, activated heavy calcium carbonate, talc, and light calcium carbonate.
[0085] In some embodiments, the polyether polyol in the B component curing agent includes polypropylene glycol; optionally, the molecular weight of the polypropylene glycol is one or more of 1000, 2000, 4000 and 8000.
[0086] In some embodiments, the polyester polyol in the B component curing agent includes phthalic anhydride polyester diol; optionally, the molecular weight of the phthalic anhydride polyester diol is one or more of 280, 350, 450 and 560.
[0087] The curing agent synthesized in this application introduces ester bonds into the molecular chain by adding low molecular weight phthalic anhydride polyester diol, which also plays a certain role in chain extension, thereby increasing the strength and rigidity of the polyurethane sealant.
[0088] In some embodiments, the isocyanate in the B component curing agent includes one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, and hexamethylene diisocyanate; optionally, the isocyanate includes one or more of TDI-80, MDI-50, MDI-100, IPDI, and HDI.
[0089] In some embodiments, the thickener comprises fumed silica.
[0090] In some embodiments, the type of plasticizer is not particularly limited and can be selected according to actual needs. The plasticizers in components A and B can be the same or different. Optionally, the plasticizer may include one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate, and dioctyl phthalate.
[0091] In some embodiments, the first catalyst includes one or more of tertiary amine catalysts and organometallic catalysts. It should be noted that the materials selected for the first catalyst in components A and B of this application can be the same or different, depending on actual needs.
[0092] In some embodiments, the tertiary amine catalyst includes one or more of aliphatic amine catalysts, ester cyclic amine catalysts, and aromatic amine catalysts. Optionally, it may include one or more of bis(2-dimethylaminoethyl) ether, N-methylmorpholine, and N,N'-dimethylpyridine.
[0093] In some embodiments, the type of organometallic catalyst is not particularly limited and can be selected according to actual needs. Optionally, it may include one or more of dibutyltin dilaurate, stannous octanoate, lead isooctanoate, zinc-bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate.
[0094] In some embodiments, the type of pigment is not particularly limited and can be selected according to actual needs. Optionally, it may include one or more of Calorie HC460, Calorie HC585, and Calorie HS461.
[0095] In some embodiments, the chain extender includes one or more of 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate, and 1,6-hexanediol;
[0096] In some embodiments, the second catalyst comprises one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc-bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate.
[0097] A second aspect of this application provides a method for preparing the two-component polyurethane sealant described in the first aspect of this application, which may include the following steps:
[0098] S10. The components contained in component A are mixed and then subjected to heat treatment and dehydration treatment to obtain component A;
[0099] S20. The dehydrated polyether polyol is reacted with isocyanate, and then the dehydrated polyester polyol is added to react to obtain the curing agent.
[0100] S30. Mix the components contained in component B to obtain component B;
[0101] S40. Mix component A and component B in a mass ratio of (10-18):1 and then cure to obtain the two-component polyurethane sealant.
[0102] In some embodiments, step S10 may further include the following steps:
[0103] S100. The polyether polyol and the filler are mixed and heated to 80°C to 120°C, and dehydrated under vacuum for 1 to 5 hours until the water content drops below 600 ppm to obtain a premix; optionally, a plasticizer is added during the mixing process of the polyether polyol and the filler.
[0104] S110. Cool the premix to below 40°C, add the first catalyst, and mix and stir evenly under vacuum conditions; optionally, a first coupling agent is also added during the mixing process of the premix and the first catalyst.
[0105] As a non-limiting example of preparing component A, polyether polyol and filler can be weighed according to the formula, and optionally, a plasticizer can also be added. Then, the mixture is put into a planetary stirred tank, stirred at a speed of 50 r / min to 500 r / min, heated to 80℃ to 120℃, and vacuum dehydrated for 1 h to 5 h until the water content is reduced to below 600 ppm. The temperature is then lowered to below 40℃, a first catalyst is added, and optionally, a first coupling agent is also added. The mixture is stirred at a speed of 50 r / min to 500 r / min under vacuum for 30 min to 120 min, and then sealed and packaged under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0106] In some embodiments, step S20 above may further include the following steps:
[0107] S200. The dehydrated polyether polyol is reacted with isocyanate at a reaction temperature of 70°C to 85°C for a reaction time of 0.5 h to 3 h under a nitrogen protective atmosphere. Optionally, the dehydrated polyether polyol is further mixed with a second catalyst.
[0108] S210, then add dehydrated polyester polyol to react, the reaction temperature is 70℃~85℃, the reaction time is 0.5h~2h, and the reaction atmosphere is nitrogen protective atmosphere;
[0109] S220, Optionally, after the dehydration-treated polyester polyol is added and reacted, a dehydration-treated chain extender is added to continue the reaction. The reaction temperature is 70℃~85℃, the reaction time is 0.5h~2h, and the reaction atmosphere is a nitrogen protective atmosphere.
[0110] As a non-limiting example of preparing component B curing agent, polyether diol is added to a reactor according to the specified ratio, and the temperature is raised to 90℃~110℃. Water is removed under vacuum for 1h~2h. The temperature is then lowered to 70℃~85℃, and isocyanate component is added. Optionally, a second catalyst is also added to the reactor. The reaction is carried out under nitrogen protection for 0.5h~3h. Then, dehydrated polyester polyol is added, and the reaction is carried out under nitrogen protection for 0.5h~2h. Optionally, dehydrated chain extender is added, and the reaction is carried out under nitrogen protection for 0.5h~2h to obtain curing agent, which is then sealed and stored for later use.
[0111] In some embodiments, step S30 above may further include the following steps:
[0112] S300. Under vacuum conditions, the curing agent and color paste are mixed evenly, then the second coupling agent is added and mixed evenly. The thickener is then added while stirring until the viscosity reaches (3 × 10⁻⁶). 4 ) mPa·s~(12×10 4 ) mPa·s; Optionally, the first catalyst and / or plasticizer are also added during the step of adding the second coupling agent.
[0113] As a non-limiting example of preparing component B, the curing agent and colorant can be weighed according to the formula and added to a planetary mixer. The mixture is stirred at a speed of 50 r / min to 500 r / min under vacuum for 0.5 h to 3 h until homogeneous. Then, the second coupling agent is added, and optionally, the first catalyst and / or plasticizer are added. The mixture is stirred at a speed of 50 r / min to 500 r / min under vacuum for 5 min to 120 min until homogeneous. Then, the thickener is added, and the mixture is stirred at a speed of 50 r / min to 500 r / min under vacuum for 30 min to 180 min until homogeneous, until the viscosity reaches (3 × 10⁻⁶). 4 ) mPa·s~(12×10 4 The solution is heated to 0.5 mPa·s and then sealed under nitrogen protection to obtain component B.
[0114] In some embodiments, the vacuum level of the vacuum condition is 0.09 MPa or higher.
[0115] In some embodiments, the stirring rate is 50 r / min to 500 r / min.
[0116] The third aspect of this application provides an application of a two-component polyurethane sealant in insulating glass, the two-component polyurethane sealant including the two-component polyurethane sealant described in the first aspect of this application or a two-component polyurethane sealant prepared according to the method described in the second aspect of this application.
[0117] Example
[0118] The following are specific embodiments, which describe the disclosure of this application in more detail. These embodiments are merely illustrative, as various modifications and variations within the scope of the disclosure of this application will be apparent to those skilled in the art. Unless otherwise stated, all parts, percentages, and ratios reported in the following embodiments are based on weight, and all reagents used in the embodiments are commercially available or synthesized by conventional methods and can be used directly without further processing, and the instruments used in the embodiments are commercially available.
[0119] The raw materials used in the following examples are from the following sources:
[0120] The polypropylene glycol manufacturer mentioned is Shandong Lanxing Dongda, with a molecular weight of 1000 and a brand name of DL-1000D; a molecular weight of 2000 and a brand name of DL-2000D; a molecular weight of 4000 and a brand name of DL-4000D; and a molecular weight of 8000 and a brand name of DL-8000D.
[0121] The polyoxypropylene triol manufacturer, Shandong Lanxing Dongda, produces the following grades: MN-300 (molecular weight 300), MN-400 (molecular weight 400), MN-500 (molecular weight 500), MN-700 (molecular weight 700), and MN-1000 (molecular weight 1000).
[0122] The filler nano-calcium carbonate is manufactured by Guangxi Huana New Material Technology Co., Ltd., grade CCS-23; the heavy calcium carbonate is manufactured by Lingyuan Xinli Calcium Industry, grade 800 mesh; the activated heavy calcium carbonate is manufactured by Jiangxi Guangyuan Chemical Co., Ltd., grade HX-1250; the talc powder is manufactured by Haiyan Rock Powder Factory, grade HY-9246; and the light calcium carbonate is manufactured by Shandong Zhongtian Mining, grade ZT501.
[0123] The thickener, fumed silica, is manufactured by Evonik, and its grade is R974.
[0124] The phthalic anhydride polyester diols mentioned are manufactured by Nanjing Jinling Stepan Chemical Co., Ltd., and have molecular weights of 280, 350, 450, and 560.
[0125] The toluene diisocyanate (TDI-80), diphenylmethane diisocyanate (MDI-50, MDI-100), isophorone diisocyanate (IPDI), and hexamethylene diisocyanate (HDI) in the isocyanates were all purchased from Wanhua Chemical Group Co., Ltd.
[0126] The plasticizers, including diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate, and dioctyl phthalate, were all purchased from Shandong Qilu Plasticizer Co., Ltd.
[0127] KH-560, KH-550, and KH-792 in the first coupling agent were all purchased from Jiangxi Chenguang New Materials Co., Ltd.; A-1170 was purchased from Momentive Advanced Materials (China) Co., Ltd.
[0128] The bis(2-dimethylaminoethyl) ether, N-methylmorpholine, and N,N'-dimethylpyridine in the tertiary amine catalyst were all purchased from Momentive Advanced Materials (China) Co., Ltd.
[0129] The dibutyltin dilaurate, stannous octate, lead isooctanoate, zinc bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate in the organometallic catalyst were all purchased from Xindian Chemical.
[0130] The pigments HC460, HC585, and HS461 in the pigment paste were all purchased from Kaller New Materials Co., Ltd.
[0131] The second coupling agent, KH-560, was purchased from Jiangxi Chenguang New Materials Co., Ltd.
[0132] The chain extenders 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate, and 1,6-hexanediol were all purchased from Aladdin.
[0133] All other raw materials not specifically mentioned are ordinary commercially available products.
[0134] Example 1
[0135] Weigh out 80g of polypropylene glycol with a molecular weight of 1000, 11g of polypropylene glycol with a molecular weight of 2000, 5g of polypropylene triol with a molecular weight of 400, 4g of polypropylene triol with a molecular weight of 1000, 300g of diisodecyl phthalate, 200g of nano-calcium carbonate, and 379.9g of activated heavy calcium carbonate. Add them to a planetary stirred tank and dehydrate for 2 hours at a speed of 300r / min, heating to 100℃ and a vacuum degree of 0.09MPa or higher until the water content drops below 600ppm. Cool down to below 40℃, add 20g of KH-550 and 0.1g of bis(2-dimethylaminoethyl) ether, and stir for 40 minutes at a speed of 300r / min and a vacuum degree of 0.09MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0136] Weigh 250g of polypropylene glycol with a molecular weight of 1000 and put it into a reaction vessel. Heat the vessel to 110℃ and remove water for 2 hours under a vacuum of 0.09MPa or higher. Cool the vessel to 85℃, add 10g of dibutyltin dilaurate, mix well, and then add 700g of HDI. React under nitrogen protection for 3 hours. Then add 10g of phthalic anhydride polyester glycol with a molecular weight of 280 after water removal and react under nitrogen protection for 1 hour. Finally, add 30g of diethylene glycol after water removal and react under nitrogen protection for 2 hours to obtain a curing agent. Seal and store the curing agent for later use.
[0137] Weigh 600g of the prepared curing agent and 280g of Kaller HS461, and add them to a planetary mixer. Stir for 3 hours at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 45g of KH-560, 5g of stannous octoate, and 20g of dioctyl phthalate. Stir for 20 minutes at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 50g of fumed silica and stir for 180 minutes at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 12 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0138] The prepared components A and B are mixed evenly at a mass ratio of 12:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0139] Example 2
[0140] Weigh out 40g of polypropylene glycol with a molecular weight of 1000, 100g of polypropylene glycol with a molecular weight of 4000, 10g of polypropylene triol with a molecular weight of 300, 148g of dioctyl phthalate, 300g of light calcium carbonate, and 400g of activated heavy calcium carbonate. Add them to a planetary stirred tank and dehydrate for 5 hours at a speed of 400 rpm and a temperature of 110°C under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool the mixture to below 40°C, add 2g of N,N'-dimethylpyridine, and stir for 60 minutes at a speed of 400 rpm and a vacuum of 0.09 MPa or higher. Seal and package the mixture under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0141] Weigh 135g of polypropylene glycol with a molecular weight of 2000 and put it into a reaction vessel. Heat the vessel to 100℃ and remove water for 1.5h under a vacuum of 0.09MPa or higher. Cool the vessel to 72℃, add 5g of zinc neodecanoate, mix well, and then add 800g of IPDI. React under nitrogen protection for 1h. Then add 40g of phthalic anhydride polyester glycol with a molecular weight of 350 after water removal and react under nitrogen protection for 2h. Finally, add 20g of ethylene glycol after water removal and react under nitrogen protection for 1.5h to obtain a curing agent. Seal and store the curing agent for later use.
[0142] Weigh 640g of the prepared curing agent and 260g of Calorie HC585, and add them to a planetary mixer. Stir at 400 rpm and a vacuum of 0.09 MPa or higher for 2 hours until homogeneous. Then add 10g of KH-560 and 50g of diisodecyl phthalate, and stir at 400 rpm and a vacuum of 0.09 MPa or higher for 40 minutes until homogeneous. Finally, add 40g of fumed silica, and stir at 400 rpm and a vacuum of 0.09 MPa or higher for 150 minutes until homogeneous and the viscosity reaches 10 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0143] The prepared components A and B are mixed evenly at a mass ratio of 11:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0144] Example 3
[0145] Weigh out 100g of polypropylene glycol with a molecular weight of 2000, 170g of polypropylene glycol with a molecular weight of 4000, 100g of polypropylene glycol with a molecular weight of 8000, 30g of polypropylene triol with a molecular weight of 500, 89.2g of diisononyl phthalate, 200g of nano-calcium carbonate, and 300g of heavy calcium carbonate. Add these ingredients to a planetary stirred tank at a speed of 200 rpm. Heat to 90°C and dehydrate under a vacuum of 0.09 MPa or higher for 3 hours until the water content drops below 600 ppm. Cool to below 40°C, add 10g of Momentive A-1170 and 0.8g of N-methylmorpholine. Stir at 200 rpm under a vacuum of 0.09 MPa or higher for 50 minutes. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0146] Weigh 150g of polypropylene glycol with a molecular weight of 1000 and 57g of polypropylene glycol with a molecular weight of 8000, and put them into a reaction vessel. Heat to 105℃ and remove water under a vacuum of 0.09MPa or higher for 2 hours. Cool down to 83℃, add 3g of bismuth isooctanoate, mix well, and then add 750g of TDI-80. React under nitrogen protection for 2.5 hours. Then add 30g of phthalic anhydride polyester glycol with a molecular weight of 450 after dehydration and react under nitrogen protection for 1.5 hours. Finally, add 10g of 1,4-butanediol after dehydration and react under nitrogen protection for 1.5 hours to obtain the curing agent, which is then sealed and stored for later use.
[0147] Weigh 670g of the prepared curing agent and 239g of Calorie HC460, and add them to a planetary mixer. Stir for 1 hour at 500 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 50g of KH-560, 10g of dibutyl phthalate, and 1g of lead isooctanoate. Stir for 5 minutes at 500 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 30g of fumed silica and stir for 30 minutes at 500 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 9 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0148] The prepared components A and B are mixed evenly at a mass ratio of 10:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0149] Example 4
[0150] Weigh out 84g of polypropylene glycol with a molecular weight of 2000, 100g of polypropylene glycol with a molecular weight of 4000, 16g of polypropylene triol with a molecular weight of 700, 170g of dibutyl phthalate, and 613.8g of talc. Add them to a planetary mixer and dehydrate for 4 hours at a speed of 100r / min, heating to 80℃ and a vacuum degree of 0.09MPa or higher until the water content drops below 600ppm. Cool down to below 40℃, add 15g of KH-792 and 1.2g of dibutyltin dilaurate, and stir for 70 minutes at a speed of 100r / min and a vacuum degree of 0.09MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0151] Weigh 80g of polypropylene glycol with a molecular weight of 4000 and put it into a reaction vessel. Heat the vessel to 90℃ and remove water for 1 hour under a vacuum of 0.09MPa or higher. Cool the vessel to 70℃ and add 900g of MDI-50. React under nitrogen protection for 1 hour. Then add 5g of phthalic anhydride polyester glycol with a molecular weight of 560 after water removal and react under nitrogen protection for 0.5 hours. Finally, add 15g of 1,6-hexanediol after water removal and react under nitrogen protection for 1 hour to obtain a curing agent. Seal and store the curing agent for later use.
[0152] Weigh 750g of the prepared curing agent and 208g of Kaller HS461, and add them to a planetary mixer. Stir for 1.5 hours at a speed of 200 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 15g of KH-560, 15g of diisononyl phthalate, and 2g of zinc-bismuth composite catalyst. Stir for 60 minutes at a speed of 200 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 10g of fumed silica and stir for 50 minutes at a speed of 200 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 3 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0153] The prepared components A and B are mixed evenly at a mass ratio of 15:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0154] Example 5
[0155] Weigh out 70g of polypropylene glycol with a molecular weight of 1000, 200g of polypropylene glycol with a molecular weight of 4000, 20g of polypropylene triol with a molecular weight of 500, 80g of diisodecyl phthalate, 100g of dibutyl phthalate, 200g of nano-calcium carbonate, and 323.3g of heavy calcium carbonate. Add them to a planetary stirred tank and dehydrate for 1 hour at a speed of 500 rpm and a temperature of 120°C under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool down to below 40°C, add 5g of KH-560 and 1.7g of zinc neodecanoate, and stir for 30 minutes at a speed of 500 rpm and a vacuum of 0.09 MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0156] Weigh 50g of polypropylene glycol with a molecular weight of 2000 and 57g of polypropylene glycol with a molecular weight of 8000, and put them into a reaction vessel. Heat to 102℃ and remove water under a vacuum of 0.09MPa or higher for 1.5h. Cool down to 85℃, add 6g of zinc-bismuth composite catalyst, mix well, and then add 844g of TDI-80. React under nitrogen protection for 0.5h. Then add 20g of phthalic anhydride polyester glycol with a molecular weight of 450 after water removal and react under nitrogen protection for 1.5h. Finally, add 23g of 1,6-hexanediol after water removal and react under nitrogen protection for 1.5h to obtain the curing agent, which is then sealed and stored for later use.
[0157] Weigh 800g of the prepared curing agent and 100g of Calorie HC585, and add them to a planetary mixer. Stir for 2.5 hours at a speed of 50 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 40g of KH-560, 37g of diisodecyl phthalate, and 3g of bismuth isooctanoate. Stir for 120 minutes at a speed of 50 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 20g of fumed silica and stir for 100 minutes at a speed of 50 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 8 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0158] The prepared components A and B are mixed evenly at a mass ratio of 14:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0159] Example 6
[0160] Weigh out 35g of polypropylene glycol with a molecular weight of 2000, 95g of polypropylene glycol with a molecular weight of 4000, 187g of polypropylene glycol with a molecular weight of 8000, 23g of polypropylene triol with a molecular weight of 700, 250g of light calcium carbonate, and 400g of activated heavy calcium carbonate. Add them to a planetary stirred tank and dehydrate for 3 hours at a speed of 300 rpm and a temperature of 100°C under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool down to below 40°C, add 4g of KH-560, 4.5g of KH-550, and 1.5g of bismuth isooctanoate. Stir for 80 minutes at a speed of 300 rpm and a vacuum of 0.09 MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0161] Weigh 25g of polypropylene glycol with a molecular weight of 2000 and 160g of polypropylene glycol with a molecular weight of 4000, and put them into a reaction vessel. Heat to 110℃ and remove water for 2 hours under a vacuum of 0.09MPa or higher. Cool down to 80℃, add 780g of MDI-100, and react for 2 hours under nitrogen protection. Then add 35g of phthalic anhydride polyester glycol with a molecular weight of 560 after water removal, and react for 2 hours under nitrogen protection to obtain a curing agent, which is then sealed and stored for later use.
[0162] Weigh 730g of the prepared curing agent and 203g of Calorie HC460, and add them to a planetary mixer. Stir for 2 hours at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 20g of KH-560, 28g of dioctyl phthalate, and 4g of zinc neodecanoate. Stir for 100 minutes at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 15g of fumed silica and stir for 80 minutes at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 6 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0163] The prepared components A and B are mixed evenly at a mass ratio of 13:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0164] Example 7
[0165] Weigh out 80g of polypropylene glycol with a molecular weight of 2000, 150g of polypropylene glycol with a molecular weight of 4000, 20g of polypropylene triol with a molecular weight of 400, 30g of dioctyl phthalate, 41g of diisononyl phthalate, 260g of nano-calcium carbonate, and 400g of activated heavy calcium carbonate. Add them to a planetary stirred tank and dehydrate for 5 hours at a speed of 50 r / min, heating to 90℃ and a vacuum degree of 0.09 MPa or higher until the water content drops below 600 ppm. Cool down to below 40℃, add 18g of KH-560 and 1g of zinc-bismuth composite catalyst, and stir for 110 minutes at a speed of 50 r / min and a vacuum degree of 0.09 MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0166] Weigh 100g of polypropylene glycol with a molecular weight of 1000 and 58g of polypropylene glycol with a molecular weight of 4000, and put them into a reaction vessel. Heat to 93℃ and remove water under a vacuum of 0.09MPa or higher for 1.5h. Cool down to 76℃, add 2g of lead isooctanoate, mix well, and then add 820g of HDI. React under nitrogen protection for 1.5h. Then add 15g of phthalic anhydride polyester glycol with a molecular weight of 350 after water removal and react under nitrogen protection for 1h. Finally, add 5g of 1,4-butanediol after water removal and react under nitrogen protection for 0.5h to obtain the curing agent, which is then sealed and stored for later use.
[0167] Weigh 850g of the prepared curing agent and 124.5g of Kaller HS461, and add them to a planetary mixer. Stir at 450 rpm and a vacuum of 0.09 MPa or higher for 0.5 hours until homogeneous. Then add 11g of KH-560 and 1.5g of dibutyltin dilaurate, and stir at 450 rpm and a vacuum of 0.09 MPa or higher for 80 minutes until homogeneous. Finally, add 13g of fumed silica, and stir at 450 rpm and a vacuum of 0.09 MPa or higher for 120 minutes until homogeneous and the viscosity reaches 5 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0168] The prepared components A and B are mixed evenly at a mass ratio of 18:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0169] Example 8
[0170] Weigh out 165g of polypropylene glycol with a molecular weight of 4000, 11g of polypropylene triol with a molecular weight of 400, 4g of polypropylene triol with a molecular weight of 500, 100g of diisodecyl phthalate, 157.5g of diisononyl phthalate, 300g of light calcium carbonate, and 250g of talc. Add them to a planetary mixer and heat to 105℃ at 250 rpm. Dehydrate for 2.5 hours under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool to below 40℃, add 12g of Momentive A-1170 and 0.5g of lead isooctanoate, and stir for 90 minutes at 250 rpm under a vacuum of 0.09 MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0171] Weigh 200g of polypropylene glycol with a molecular weight of 1000 and 28g of polypropylene glycol with a molecular weight of 8000, and put them into a reaction vessel. Heat to 98℃ and remove water for 2 hours under a vacuum of 0.09MPa or higher. Cool down to 83℃, add 8g of stannous octoate, mix well, and then add 730g of TDI-80. React under nitrogen protection for 2 hours. Then add 8g of phthalic anhydride polyester glycol with a molecular weight of 280 after water removal and react under nitrogen protection for 0.5 hours. Finally, add 26g of diethylene glycol after water removal and react under nitrogen protection for 2 hours to obtain the curing agent, which is then sealed and stored for later use.
[0172] Weigh 780g of the prepared curing agent and 130g of Calorie HC585, and add them to a planetary mixer. Stir for 1 hour at a speed of 250 rpm and a vacuum of 0.09 MPa or higher until the mixture is homogeneous. Then add 30g of KH-560, 45g of diisononyl phthalate, and 2g of N-methylmorpholine. Stir for 15 minutes at a speed of 250 rpm and a vacuum of 0.09 MPa or higher until the mixture is homogeneous. Finally, add 13g of fumed silica and stir for 60 minutes at a speed of 250 rpm and a vacuum of 0.09 MPa or higher until the mixture is homogeneous and the viscosity reaches 5 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0173] The prepared components A and B are mixed evenly at a mass ratio of 16:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0174] Example 9
[0175] Weigh out 100g of polypropylene glycol with a molecular weight of 1000, 240g of polypropylene glycol with a molecular weight of 8000, 10g of polypropylene triol with a molecular weight of 500, 20g of polypropylene triol with a molecular weight of 1000, 60g of dioctyl phthalate, 55g of dibutyl phthalate, 300g of calcium carbonate, and 200g of talc. Add them to a planetary mixer and heat to 115℃ at 320 rpm. Dehydrate for 3.5 hours under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool to below 40℃, add 14g of KH-792 and 1g of stannous octoate, and stir for 120 minutes at 320 rpm under a vacuum of 0.09 MPa or higher. Seal and package under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.
[0176] Weigh 50g of polypropylene glycol with a molecular weight of 2000 and 50g of polypropylene glycol with a molecular weight of 4000, and put them into a reaction vessel. Heat to 95℃ and remove water under a vacuum of 0.09MPa or higher for 1.5h. Cool down to 73℃, add 1g of dibutyltin dilaurate, mix well, and then add 870g of MDI-50. React under nitrogen protection for 2.5h. Then add 25g of phthalic anhydride polyester glycol with a molecular weight of 560 after water removal and react under nitrogen protection for 1.5h. Finally, add 4g of 1,6-hexanediol after water removal and react under nitrogen protection for 0.5h to obtain the curing agent, which is then sealed and stored for later use.
[0177] Weigh 820g of the prepared curing agent and 150g of Calorie HC460, and add them to a planetary mixer. Stir for 2.5 hours at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 10g of KH-560, 1g of N,N'-dimethylpyridine, and 1g of bis(2-dimethylaminoethyl) ether. Stir for 50 minutes at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 18g of fumed silica and stir for 90 minutes at 150 rpm and a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 7 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.
[0178] The prepared components A and B are mixed evenly at a mass ratio of 10:1 and cured at room temperature to obtain a two-component polyurethane sealant.
[0179] Comparative Example 1
[0180] The preparation method of Comparative Example 1 is similar to that of Example 4, except that component A does not contain polyoxypropylene triol.
[0181] Comparative Example 2
[0182] The preparation method of Comparative Example 2 is similar to that of Example 4, except that the curing agent used in Component B is Covestro DESMODUR E22.
[0183] The two-component polyurethane sealants prepared in Examples 1-9 and Comparative Examples 1-2 were subjected to relevant performance tests, and the test results are shown in Table 1 below. All performance tests were conducted in accordance with the test standards in GB / T 29755-2013.
[0184] Table 1
[0185]
[0186] As shown in Table 1 above, the performance of the two-component polyurethane sealant prepared in this application meets and exceeds all the requirements of GB / T 29755-2013 standard. Under standard test conditions, this sealant exhibits high tensile bond strength, good elasticity, and no bond failure. After water and UV treatment, the tensile bond strength decreases by 25%–30%, while the elongation at maximum tensile bond strength increases by 90%–100%, with no bond failure. After hot air aging, the tensile bond strength increases slightly, while the elongation at maximum tensile bond strength remains unchanged, with no bond failure. The water vapor transmission rate of this sealant is within 3 g / (m²). 2 ·d)~5g / (m 2 ·d).
[0187] In Comparative Example 1, which did not contain polyoxypropylene triol, although the sealant still met all the requirements of GB / T29755-2013 standard, its performance changed significantly due to the lack of a cross-linked structure: compared with Example 4, the tensile bond strength decreased by 35%, the water vapor transmission rate increased by 88.9%, and the sealant performance decreased.
[0188] Comparative Example 2, which used Covestro DESMODUR E22 as the curing agent in component B, lacked chain extenders and had a low molecular weight, failing to meet the performance requirements of GB / T 29755-2013 standard for tensile bond strength, tensile bond strength after water UV treatment, tensile bond strength after heat aging, and bond failure area. In Comparative Example 4, the tensile bond strength decreased by 42%, the water vapor transmission rate increased by 100%, and the sealant performance deteriorated.
[0189] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0190] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this patent application should be determined by the appended claims.
Claims
1. A two-component polyurethane sealant, characterized in that, It includes component A and component B, wherein, Component A comprises the following raw materials by mass percentage: Polyether polyols, 10%~40%; Filler, 50%~70%; First adjuvant, 0.01%~32.2%; Component B comprises the following raw materials by mass percentage: Hardener, 60%~85%; Thickener, 1%~5%; Second adjuvant, 11%~38.5%; The curing agent in component B comprises the following raw materials by mass percentage: Isocyanates, 70%~90%; Polyether polyols, 8%~25%; Polyester polyols, 0.5%~4%; Third adjuvant, 0-4%; Based on the total mass of the curing agent in component B, the third auxiliary agent comprises the following raw materials by mass percentage: chain extender, 0-3%; second catalyst, 0-1%; the polyester polyol in the curing agent of component B includes phthalic anhydride polyester diol. The method for preparing the curing agent includes: reacting a dehydrated polyether polyol, a second catalyst, and isocyanate at a reaction temperature of 70℃~85℃ for 0.5h~3h under a nitrogen protective atmosphere; then adding a dehydrated polyester polyol and reacting at a reaction temperature of 70℃~85℃ for 0.5h~2h under a nitrogen protective atmosphere; finally adding a dehydrated chain extender and continuing the reaction at a reaction temperature of 70℃~85℃ for 0.5h~2h under a nitrogen protective atmosphere. The mass ratio of component A to component B is (10~18):
1.
2. The two-component polyurethane sealant according to claim 1, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) Based on the total mass of component A, the first adjuvant comprises the following raw materials by mass percentage: Plasticizer, 0~30%; First catalyst, 0.01%~0.2%; First coupling agent, 0~2%; (2) Based on the total mass of component B, the second auxiliary agent comprises the following raw materials by mass percentage: Color paste, 10%~28%; second coupling agent, 1%~5%; first catalyst, 0~0.5%; plasticizer, 0~5%.
3. The two-component polyurethane sealant according to claim 1 or 2, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) The polyether polyol in component A includes polyoxypropylene glycol and / or polyoxypropylene triol; (2) The filler includes one or more of nano-calcium carbonate, heavy calcium carbonate, activated heavy calcium carbonate, talc, and light calcium carbonate; (3) The polyether polyol in the curing agent of component B includes polyoxypropylene glycol; (4) The isocyanate in the curing agent of component B includes one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate; (5) The thickener of component B includes fumed silica.
4. The two-component polyurethane sealant according to claim 3, characterized in that, The polyoxypropylene glycol in component A has a molecular weight of one or more of 1000, 2000, 4000 and 8000.
5. The two-component polyurethane sealant according to claim 3, characterized in that, The molecular weight of the polyoxypropylene triol in component A is one or more of 300, 400, 500, 700 and 1000.
6. The two-component polyurethane sealant according to claim 3, characterized in that, The polyoxypropylene glycol in the curing agent of component B has a molecular weight of one or more of 1000, 2000, 4000 and 8000.
7. The two-component polyurethane sealant according to claim 3, characterized in that, The phthalic anhydride polyester diol in the curing agent of component B has a molecular weight of one or more of 280, 350, 450 and 560.
8. The two-component polyurethane sealant according to claim 2, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) The plasticizer includes one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate and dioctyl phthalate; (2) The first catalyst includes one or more of tertiary amine catalysts and organometallic catalysts; (3) The first coupling agent includes one or more of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-aminopropyltriethoxysilane, bis-(γ-trimethoxysilylpropyl)amine and N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane.
9. The two-component polyurethane sealant according to claim 8, characterized in that, The tertiary amine catalysts include one or more of aliphatic amine catalysts, ester cyclic amine catalysts, and aromatic amine catalysts.
10. The two-component polyurethane sealant according to claim 8, characterized in that, The organometallic catalyst includes one or more of dibutyltin dilaurate, stannous octanoate, lead isooctanoate, zinc-bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate.
11. The two-component polyurethane sealant according to claim 2, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) The color paste includes one or more of Calorie HC460, Calorie HC585 and Calorie HS461; (2) The second coupling agent includes γ-(2,3-epoxypropoxy)propyltrimethoxysilane.
12. The two-component polyurethane sealant according to claim 2, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) The chain extender includes one or more of 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate and 1,6-hexanediol; (2) The second catalyst includes one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc bismuth composite catalyst, bismuth isooctanoate and zinc neodecanoate.
13. A method for preparing the two-component polyurethane sealant according to any one of claims 1-12, characterized in that, include: The components contained in component A are mixed and then subjected to heat treatment and dehydration treatment to obtain component A; The dehydrated polyether polyol, a second catalyst, and isocyanate are reacted at a temperature of 70°C to 85°C for 0.5 to 3 hours under a nitrogen protective atmosphere. Then, a dehydrated polyester polyol is added and reacted at the same temperature for 0.5 to 2 hours under a nitrogen protective atmosphere. Finally, a dehydrated chain extender is added and the reaction continues at 70°C to 85°C for 0.5 to 2 hours under a nitrogen protective atmosphere to obtain the curing agent. The components contained in component B are mixed to obtain component B; The two-component polyurethane sealant is obtained by mixing component A and component B at a mass ratio of (10~18):1 and then curing.
14. The method according to claim 13, characterized in that, The step of mixing the components in component A and then subjecting them to heat treatment and dehydration includes: The polyether polyol and the filler are mixed and heated to 80°C~120°C, and dehydrated under vacuum for 1h~5h until the water content drops below 600ppm to obtain a premix. The premixed material is cooled to below 40°C, the first catalyst is added, and the mixture is stirred evenly under vacuum conditions.
15. The method according to claim 14, characterized in that, A plasticizer is also added during the mixing process of the polyether polyol and the filler.
16. The method according to claim 14, characterized in that, A first coupling agent is also added during the mixing process of the premix and the first catalyst.
17. The method according to claim 14, characterized in that, The mixing process of the components contained in component B includes: After the curing agent and color paste are mixed evenly under vacuum conditions, the second coupling agent is added and mixed evenly. The thickener is then added while stirring until the viscosity reaches (3 × 10⁻⁶). 4 ) mPa·s ~(12×10 4 )mPa·s.
18. The method according to claim 17, characterized in that, The first catalyst and / or plasticizer are also added during the step of adding the second coupling agent.
19. The method according to claim 14 or 17, characterized in that, The method satisfies at least one of the following conditions: (1) The vacuum degree of the vacuum condition is above 0.09 MPa; (2) The stirring rate of the stirring is 50r / min to 500r / min.
20. An application of a two-component polyurethane sealant in insulating glass, characterized in that, The two-component polyurethane sealant includes the two-component polyurethane sealant according to any one of claims 1-12 or the two-component polyurethane sealant prepared by the method according to any one of claims 13-19.
Citation Information
Patent Citations
Fast-cured bi-component polyurethane structural adhesive and its preparation method
CN103834344A
Polyurethane adhesive for compositing two-component PVC plate
CN105925236A
Two-component solvent-free polyurethane adhesive and preparation method thereof
CN111234757A