Two-component polyurethane sealant, method for preparing the same and use thereof

Abstract

The application provides a two-component polyurethane sealant and a preparation method and application thereof. The two-component polyurethane sealant comprises an A component and a B component. The A component comprises the following raw materials in percentage by mass: polyether polyol, 10-40%; chain extender, 1-3%; filler, 50-70%; first auxiliary agent, 5.01-36.5%; the B component comprises the following raw materials in percentage by mass: curing agent, 60-85%; thickening agent, 1-5%; second auxiliary agent, 10-38.5%; and the mass ratio of the A component to the B component is (1-4):1. The two-component polyurethane sealant provided by the application can be well bonded with glass and has high strength without primer.

Description

Technical Field

[0001] This application relates to the field of adhesive materials technology, and in particular to a two-component polyurethane sealant, its preparation method, and its application. Background Technology

[0002] Sealant is a material used to fill gaps (holes, seams, etc.). Elastic sealant combines both bonding and sealing functions. Sealant used in double-glazed windows is a special product used in the construction industry. Double-glazed windows are window glass products consisting of two panes of glass sealed around the edges, with dry air or a vacuum filling the space between them. They have excellent thermal insulation properties and are mainly used for doors and windows. The mainstream manufacturing process for double-sealed insulated glass uses butyl rubber for the first seal and polysulfide (PS), silicone (SR), or polyurethane (PU) elastic sealant for the second seal.

[0003] Currently, the mainstream elastic sealant used in insulated glass is silicone sealant, which has good weather resistance and is easy to apply. However, its long-term airtightness is generally poor, and it is prone to problems such as small-molecule oil seepage, large price fluctuations, and market instability. Polysulfide sealant has good long-term airtightness and excellent performance, but it has a strong odor during construction, which may affect the health of construction workers. Polyurethane sealant is an environmentally friendly material with stable raw material prices, low water vapor transmission rate and water absorption rate, and good airtightness. However, most polyurethane sealants currently on the market require a primer to ensure good adhesion to the glass, and their strength is not high. Summary of the Invention

[0004] Based on this, this application provides a two-component polyurethane sealant, its preparation method and application, which can achieve good adhesion and high strength to glass without the need for a primer.

[0005] 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 weight percentage:

[0006] Polyether polyols, 10%–40%;

[0007] Chain extender, 1%–3%;

[0008] Filler, 50%–70%;

[0009] First adjuvant, 5.01%–36.5%;

[0010] Component B comprises the following raw materials by mass percentage:

[0011] Hardener, 60%–85%;

[0012] Thickener, 1%–5%;

[0013] Second adjuvant, 10%–38.5%;

[0014] The mass ratio of component A to component B is (1-4):1.

[0015] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:

[0016] (1) In component A, the first auxiliary agent comprises the following raw materials by mass percentage:

[0017] Plasticizer, 5%–35%; Catalyst, 0.01%–0.5%; First coupling agent, 0%–1%;

[0018] (2) In component B, the second auxiliary agent comprises the following raw materials by mass percentage:

[0019] Color paste, 10%–28%; second coupling agent, 0%–5%; catalyst, 0%–0.5%; plasticizer, 0%–5%.

[0020] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:

[0021] (1) The polyether polyol includes polyoxypropylene glycol.

[0022] Optionally, the molecular weight of the polyoxypropylene glycol is one or more of 1000, 2000, 4000 and 8000;

[0023] (2) The chain extender includes one or more of 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate and 1,6-hexanediol;

[0024] (3) The filler includes one or more of nano calcium carbonate, heavy calcium carbonate, activated heavy calcium carbonate, talc and light calcium carbonate;

[0025] (4) The curing agent includes MDI prepolymer.

[0026] Optionally, the MDI prepolymer includes one or more of Covestro E22 and Covestro E23.

[0027] (5) The thickener includes fumed silica.

[0028] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:

[0029] (1) 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;

[0030] Optionally, the first coupling agent includes one or more of KH-560, KH-550, Momentive A-1170, and KH-792;

[0031] (2) The plasticizer includes one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate and dioctyl phthalate;

[0032] (3) The catalyst includes one or more of tertiary amine catalysts and organometallic catalysts;

[0033] Optionally, the tertiary amine catalyst includes one or more of aliphatic amine catalysts, ester cyclic amine catalysts, and aromatic amine catalysts;

[0034] Optionally, the organometallic catalyst includes one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc-bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate.

[0035] In some embodiments of this application, the two-component polyurethane sealant satisfies at least one of the following conditions:

[0036] (1) The color paste includes one or more of Calorie HC460, Calorie HC585 and Calorie HS461;

[0037] (2) The second coupling agent includes γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

[0038] Optionally, the second coupling agent includes KH-560;

[0039] 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:

[0040] The components contained in component A are mixed and then subjected to heat treatment and dehydration treatment to obtain component A;

[0041] The components contained in component B are mixed to obtain component B;

[0042] The two-component polyurethane sealant is obtained by mixing component A and component B in a mass ratio of (1-4):1 and then curing them.

[0043] 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:

[0044] The polyether polyol, the plasticizer, the filler and the chain extender 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.

[0045] The premix is ​​cooled to below 40°C, and the catalyst is added and mixed and stirred evenly under vacuum conditions.

[0046] Optionally, the first coupling agent is also added during the mixing process of the premix and the catalyst.

[0047] In some embodiments of this application, the mixing process of the components contained in component B includes:

[0048] The curing agent and the color paste are mixed under vacuum conditions, and the thickener is added while stirring until the viscosity reaches (3×10⁻⁶). 4 ) mPa·s~(12×10 4 ) mPa·s;

[0049] Optionally, at least one of the second coupling agent, the catalyst, and the plasticizer may be added during the mixing step of adding the curing agent and the color paste.

[0050] In some embodiments of this application, the method satisfies at least one of the following conditions:

[0051] (1) The vacuum degree of the vacuum condition is above 0.09 MPa;

[0052] (2) The stirring rate in the stirring state is 50 r / min to 500 r / min.

[0053] 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.

[0054] The two-component polyurethane sealant provided in this application allows for the adjustment of the molecular weight of the final reaction product by adding a chain extender and adjusting the mass percentage of the chain extender, thereby controlling the molecular weight of the final reaction product within a specific and suitable range. By controlling the molecular weight of the two-component polyurethane sealant within a suitable range, the interfacial adhesion between the sealant and the glass can be made greater than the cohesive force of the sealant, thus achieving cohesive failure and ensuring good adhesion performance between the sealant and the glass even without a primer. Detailed Implementation

[0055] 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.

[0056] 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.

[0057] 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.

[0058] 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.

[0059] 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%; chain extender, 1%–3%; filler, 50%–70%; and a first additive, 5.01%–36.5%; and component B comprises the following raw materials by mass percentage: curing agent, 60%–85%; thickener, 1%–5%; and a second additive, 10%–38.5%; and the mass ratio of component A to component B is (1–4):1.

[0060] The two-component polyurethane sealant provided in this application, by adding a chain extender and adjusting the mass percentage of the chain extender, can effectively leverage the synergistic effect between the chain extender and the polyether polyol, thereby adjusting the molecular weight of the final reaction product and controlling it within a specific suitable range. By controlling the molecular weight of the two-component polyurethane sealant within a suitable range, the interfacial adhesion force between the sealant and glass can be made greater than the cohesive force of the sealant, thus achieving cohesive breakdown and ensuring good adhesion performance between the sealant and glass even without a primer.

[0061] In some embodiments, the first additive in component A comprises the following raw materials by mass percentage: plasticizer, 5% to 35%; catalyst, 0.01% to 0.5%; and first coupling agent, 0% to 1%.

[0062] 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, 0% to 5%; catalyst, 0% to 0.5%; plasticizer, 0% to 5%.

[0063] 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.

[0064] In some embodiments, the second coupling agent comprises γ-(2,3-epoxypropoxy)propyltrimethoxysilane. Optionally, the second coupling agent comprises KH-560.

[0065] 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, which is beneficial for achieving a primerless application.

[0066] In some embodiments, the polyether polyol comprises polypropylene glycol. Optionally, the polypropylene glycol has a molecular weight of one or more of 1000, 2000, 4000, and 8000.

[0067] In some embodiments, the chain extender includes one or more of 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate, and 1,6-hexanediol.

[0068] In this application, the type of filler is not particularly limited and can be selected according to actual needs. Optionally, the filler may include one or more of nano-calcium carbonate, heavy calcium carbonate, activated heavy calcium carbonate, talc, and light calcium carbonate.

[0069] In some embodiments, the curing agent comprises an MDI prepolymer. Optionally, the MDI prepolymer comprises one or more of Covestro E22 and Covestro E23.

[0070] In some embodiments, the thickener comprises fumed silica.

[0071] In this application, the type of plasticizer is not particularly limited and can be selected according to actual needs. Optionally, the plasticizer may include one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate, and dioctyl phthalate.

[0072] It is understood that the types of plasticizers in component A and component B may be the same or different.

[0073] In some embodiments, the catalyst includes one or more of tertiary amine catalysts and organometallic catalysts.

[0074] 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.

[0075] 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.

[0076] It is understood that the catalyst types in component A and component B may be the same or different.

[0077] 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.

[0078] 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:

[0079] S10. The components contained in component A are mixed and then subjected to heat treatment and dehydration treatment to obtain component A;

[0080] S20. Mix the components contained in component B to obtain component B;

[0081] S30. Mix component A and component B in a mass ratio of (1-4):1 and then cure to obtain the two-component polyurethane sealant.

[0082] In some embodiments, step S10 may further include the following steps:

[0083] S100. Mix the polyether polyol, the plasticizer, the filler and the chain extender and heat to 80°C to 120°C. Dehydrate under vacuum for 1 hour to 5 hours until the water content is reduced to below 600 ppm to obtain a premix.

[0084] S110. Cool the premix to below 40°C, add the catalyst, and mix and stir evenly under vacuum conditions; optionally, the first coupling agent is also added during the mixing process of the premix and the catalyst.

[0085] As a non-limiting example of preparing component A, polyether polyol, plasticizer, filler and chain extender can be weighed according to the formula, and then put into a planetary stirred tank. The stirring speed is 50 r / min to 500 r / min, the temperature is raised to 80℃ to 120℃, and the water content is reduced to below 600 ppm under vacuum for 1 h to 5 h. The temperature is then lowered to below 40℃, a catalyst is added, and optionally a first coupling agent is added. The stirring speed is 50 r / min to 500 r / min, and the stirring is carried out under vacuum for 30 min to 120 min. The mixture is then sealed and packaged under nitrogen protection to obtain component A, which has a viscous appearance and uniform texture.

[0086] In some embodiments, step S20 above may further include the following steps:

[0087] S200. Mix the curing agent and the color paste under vacuum conditions, and add the thickener while stirring until the viscosity reaches (3×10). 4 ) mPa·s~(12×10 4 ) mPa·s;

[0088] Optionally, at least one of the second coupling agent, the catalyst, and the plasticizer may be added during the mixing step of adding the curing agent and the color paste.

[0089] As a non-limiting example of preparing component B, the curing agent and color paste 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. Optionally, at least one of a second coupling agent, a catalyst, and a plasticizer can be 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, a thickener is added. 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.

[0090] In some embodiments, the vacuum level of the vacuum condition is 0.09 MPa or higher.

[0091] In some embodiments, the stirring rate of the stirring state is 50 r / min to 500 r / min.

[0092] 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.

[0093] Example

[0094] 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.

[0095] The raw materials used in the following examples are from the following sources:

[0096] 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.

[0097] The chain extenders 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate, and 1,6-hexanediol were all purchased from Aladdin.

[0098] The plasticizers diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate, and dioctyl phthalate were all purchased from Shandong Qilu Plasticizer Co., Ltd.

[0099] 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.

[0100] The first coupling agents KH-560, KH-550, and KH-792 were all purchased from Jiangxi Chenguang New Materials Co., Ltd.; A-1170 was purchased from Momentive Advanced Materials (China) Co., Ltd.

[0101] The tertiary amine catalysts bis(2-dimethylaminoethyl) ether, N-methylmorpholine, and N,N'-dimethylpyridine were all purchased from Momentive Advanced Materials (China) Co., Ltd.; the organometallic catalysts, including dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc bismuth composite catalyst, bismuth isooctanoate, and zinc neodecanoate, were all purchased from Newdian Chemicals.

[0102] The curing agent is manufactured by Covestro, and its brands are DESMODUR E22 and DESMODUR E23.

[0103] The color pastes HC460, HC585, and HS461 were all purchased from Kaller New Materials Co., Ltd.

[0104] The second coupling agent, KH-560, was purchased from Jiangxi Chenguang New Materials Co., Ltd.

[0105] The thickener, fumed silica, is manufactured by Evonik, and its grade is R974.

[0106] All other raw materials not specifically mentioned are ordinary commercially available products.

[0107] Example 1

[0108] Weigh out 55g of polypropylene glycol with a molecular weight of 1000, 45g of polypropylene glycol with a molecular weight of 8000, 350g of diisodecyl phthalate, 200g of nano-calcium carbonate, 310g of activated heavy calcium carbonate, and 30g of ethylene glycol. Add them to a planetary stirred tank and dehydrate for 1 hour at a speed of 100r / 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 5g of KH-560 and 5g of bis(2-dimethylaminoethyl) ether, and stir for 100 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.

[0109] Weigh out 500g of MDI prepolymer DESMODUR E22, 100g of MDI prepolymer DESMODUR E23, and 280g of Calorie HC460, and add them to a planetary mixer. Stir for 2 hours at 100 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 25g of KH-560, 5g of stannous octoate, and 40g of dioctyl phthalate. Stir for 60 minutes at 100 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 50g of fumed silica and stir for 60 minutes at 100 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.

[0110] The prepared components A and B are mixed evenly at a mass ratio of 1:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0111] Example 2

[0112] Weigh out 140g of polypropylene glycol with a molecular weight of 1000, 100g of polypropylene glycol with a molecular weight of 2000, 60g of polypropylene glycol with a molecular weight of 8000, 184g of dibutyl phthalate, 310g of light calcium carbonate, 190g of heavy calcium carbonate, and 12g of 1,4-butanediol. Add them to a planetary stirred tank and dehydrate for 2 hours at a speed of 50r / 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 3g of KH-550 and 1g of N,N'-dimethylpyridine, and stir for 120 minutes at a speed of 50r / 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.

[0113] Weigh out 500g of MDI prepolymer DESMODUR E22, 250g of MDI prepolymer DESMODUR E23, and 177g of Kaller HS461, and add them to a planetary stirred tank. Stir at 500 rpm and a vacuum of 0.09 MPa or higher for 0.5 hours until homogeneous. Then add 50g of KH-560, 1g of lead isooctanoate, and 2g of zinc-bismuth composite catalyst. Stir at 500 rpm and a vacuum of 0.09 MPa or higher for 5 minutes until homogeneous. Finally, add 20g of fumed silica and stir at 50 rpm and a vacuum of 0.09 MPa or higher for 180 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.

[0114] The prepared components A and B are mixed evenly at a mass ratio of 2:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0115] Example 3

[0116] Weigh out 200g of polypropylene glycol with a molecular weight of 2000, 200g of polypropylene glycol with a molecular weight of 4000, 77g of dioctyl phthalate, 500g of talc, and 10g of 1,6-hexanediol. Add them to a planetary mixer and dehydrate for 2.5h at a speed of 500r / min, heating to 120℃ and a vacuum degree of 0.09MPa or higher until the water content drops below 600ppm. Cool down to below 40℃, add 10g of Momentive A-1170, 1g of N-methylmorpholine, and 2g of dibutyltin dilaurate. Stir for 30min at a speed of 500r / 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.

[0117] Weigh out 400g of MDI prepolymer DESMODUR E22, 450g of MDI prepolymer DESMODUR E23, and 100g of Calorie HC585, and add them to a planetary mixer. Stir for 3 hours at 50 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 10g of KH-560 and 10g of diisononyl phthalate, and stir for 120 minutes at 50 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 7 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.

[0118] The prepared components A and B are mixed evenly at a mass ratio of 4:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0119] Example 4

[0120] Weigh out 90g of polypropylene glycol with a molecular weight of 1000, 60g of polypropylene glycol with a molecular weight of 4000, 112g of diisononyl phthalate, 320g of nano-calcium carbonate, 380g of heavy calcium carbonate, and 28g of diethylene glycol. Add them to a planetary stirred tank and dehydrate for 5 hours at a speed of 300r / min, heating to 90℃ and a vacuum degree of 0.09MPa or higher until the water content drops below 600ppm. Cool down to below 40℃, add 7g of KH-792 and 3g of zinc neodecanoate, and stir for 60 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.

[0121] Weigh 650g of MDI prepolymer DESMODUR E23 and 257g of Kaller HS461, and add them to a planetary mixer. Stir for 2 hours at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 30g of KH-560, 2g of bis(2-dimethylaminoethyl) ether, 1g of N,N'-dimethylpyridine, and 50g of dibutyl phthalate. Stir for 70 minutes at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 10g of fumed silica and stir for 50 minutes at 250 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.

[0122] The prepared components A and B are mixed evenly at a mass ratio of 2:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0123] Example 5

[0124] Weigh out 140g of polypropylene glycol with a molecular weight of 1000, 40g of polypropylene glycol with a molecular weight of 2000, 40g of polypropylene glycol with a molecular weight of 4000, 144.9g of dioctyl phthalate, 260g of light calcium carbonate, 340g of heavy calcium carbonate, 12g of ethylene glycol, and 14g of 1,6-hexanediol. Add them to a planetary stirred tank and dehydrate for 4 hours at a speed of 200 rpm and a temperature of 100°C or higher under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool down to below 40°C, add 9g of KH-550 and 0.1g of bismuth isooctanoate, and stir for 80 minutes at a speed of 200 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.

[0125] Weigh out 380g of MDI prepolymer DESMODUR E22, 320g of MDI prepolymer DESMODUR E23, and 220g of Calorie HC460, and add them to a planetary mixer. Stir for 1.5 hours at 200 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 30g of KH-560, 2g of N-methylmorpholine, 3g of dibutyltin dilaurate, and 15g of diisodecyl phthalate. Stir for 80 minutes at 200 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 30g of fumed silica and stir for 80 minutes at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. The viscosity should reach 7.5 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.

[0126] The prepared components A and B are mixed evenly at a mass ratio of 1.5:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0127] Example 6

[0128] Weigh out 30g of polypropylene glycol with a molecular weight of 2000, 120g of polypropylene glycol with a molecular weight of 4000, 100g of polypropylene glycol with a molecular weight of 8000, 50g of diisodecyl phthalate, 310g of nano-calcium carbonate, 362g of activated heavy calcium carbonate, and 20g of 1,6-hexanediol. Add them to a planetary stirred tank and dehydrate for 4.5h at a speed of 300r / min, heating to 110℃ and a vacuum degree of 0.09MPa or higher until the water content drops below 600ppm. Cool down to below 40℃, add 6g of Momentive A-1170, 1g of lead isooctanoate, and 1g of zinc bismuth composite catalyst. Stir for 70min 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.

[0129] Weigh 720g of MDI prepolymer DESMODUR E22 and 186g of Kaller HC585, and add them to a planetary mixer. Stir for 1 hour at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 20g of KH-560, 4g of zinc neodecanoate, and 40g of dibutyl phthalate. Stir for 90 minutes at 300 rpm and a vacuum of 0.09 MPa or higher until homogeneous. Then add 30g of fumed silica and stir for 100 minutes at 200 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.

[0130] The prepared components A and B are mixed evenly at a mass ratio of 2.3:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0131] Example 7

[0132] Weigh out 200g of polypropylene glycol with a molecular weight of 2000, 150g of polypropylene glycol with a molecular weight of 4000, 100g of dibutyl phthalate, 200g of light calcium carbonate, 331g of heavy calcium carbonate, 5g of ethylene glycol, and 10g of 1,6-hexanediol. Add them to a planetary mixer and heat to 100°C at a speed of 100 rpm. Dehydrate for 3 hours under a vacuum of 0.09 MPa or higher until the water content drops below 600 ppm. Cool to below 40°C, add 4g of stannous octoate, and stir for 90 minutes at a speed of 100 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.

[0133] Weigh out 200g of MDI prepolymer DESMODUR E22, 600g of MDI prepolymer DESMODUR E23, and 127g of Calorie HC460. Add them to a planetary mixer and stir for 2 hours at 100 rpm under a vacuum of 0.09 MPa or higher until homogeneous. Then add 3g of bismuth isooctanoate and 30g of diisodecyl phthalate. Stir for 30 minutes at 100 rpm under a vacuum of 0.09 MPa or higher until homogeneous. Finally, add 40g of fumed silica and stir for 120 minutes at 100 rpm under a vacuum of 0.09 MPa or higher until homogeneous and the viscosity reaches 10.5 × 10⁻⁶. 4 The solution is heated to mPa·s and then sealed under nitrogen protection to obtain component B.

[0134] The prepared components A and B are mixed evenly at a mass ratio of 3:1 and cured at room temperature to obtain a high-strength, primerless two-component polyurethane sealant.

[0135] Comparative Example 1

[0136] The preparation method of Comparative Example 1 is similar to that of Example 3, except that the raw materials of Component A do not contain chain extenders.

[0137] Comparative Example 2

[0138] The preparation method of Comparative Example 2 is similar to that of Example 3, except that the mass percentage of chain extender in the raw material of component A is 0.1%.

[0139] Comparative Example 3

[0140] The preparation method of Comparative Example 3 is similar to that of Example 3, except that the mass percentage of chain extender in the raw material of component A is 8%.

[0141] The two-component polyurethane sealants prepared in Examples 1-7 and Comparative Examples 1-3 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.

[0142] Table 1

[0143]

[0144] As shown in Table 1 above, this two-component polyurethane sealant exhibits high tensile bond strength. Examples with added coupling agents show no bond failure, while Example 7 without coupling agents shows partial bond failure, but still meets the bond failure requirements of GB / T29755-2013. After water and UV treatment, the tensile bond strength decreases by 45%-50%, while the elongation at maximum tensile bond strength increases by 80%-90%. After hot air aging, the performance remains unchanged. The water vapor transmission rate of this two-component polyurethane sealant is (5-7) g / (m²). 2 ·d).

[0145] Comparative Example 1, which did not contain a chain extender, did not meet the performance requirements of GB / T 29755-2013 standard in terms of tensile bond strength, elongation, and bond failure area. After water UV treatment, the tensile bond strength decreased by 60%, the elongation at maximum tensile bond strength increased by 100%, and the bond failure area decreased by 20%. After hot air aging, the performance remained unchanged.

[0146] Comparative Example 3, with an excess of chain extender, exhibited high tensile bond strength, but its elongation and bond failure area at maximum tensile bond strength failed to meet the performance requirements of GB / T 29755-2013 standard. After water-UV treatment, the tensile bond strength decreased by 55%, while the elongation at maximum tensile bond strength increased by 66%, resulting in complete bond failure. After hot air aging, the performance remained unchanged.

[0147] 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.

[0148] 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 for insulating glass, 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%; Chain extender, 1%~1.5%; Filler, 50%~70%; First adjuvant, 5.01%~36.5%; Component B comprises the following raw materials by mass percentage: Hardener, 60%~85%; Thickener, 1%~5%; Second adjuvant, 10%~38.5%; The mass ratio of component A to component B is (1~4):1; The chain extender is one or more selected from 1,4-butanediol, ethylene glycol, diethylene glycol monohydrate, and 1,6-hexanediol; the curing agent includes MDI prepolymer. Based on the total mass of component A, the first auxiliary agent comprises the following raw materials by mass percentage: plasticizer, 5%~35%; catalyst, 0.01%~0.5%; first coupling agent, 0%~1%; 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, 0%~5%; catalyst, 0%~0.5%; plasticizer, 0%~5%.

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) The polyether polyol includes polyoxypropylene glycol; (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 MDI prepolymer includes one or more of Covestro E22 and Covestro E23; (4) The thickener includes fumed silica.

3. The two-component polyurethane sealant according to claim 2, characterized in that, The polyoxypropylene glycol has a molecular weight of one or more of 1000, 2000, 4000 and 8000.

4. The two-component polyurethane sealant according to any one of claims 1-3, characterized in that, The two-component polyurethane sealant meets at least one of the following conditions: (1) 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; (2) The plasticizer includes one or more of diisodecyl phthalate, diisononyl phthalate, dibutyl phthalate and dioctyl phthalate; (3) The catalyst includes one or more of tertiary amine catalysts and organometallic catalysts.

5. The two-component polyurethane sealant according to claim 4, characterized in that, One or more of the following conditions must be met: (1) The tertiary amine catalyst includes one or more of aliphatic amine catalysts, ester cyclic amine catalysts, and aromatic amine catalysts; (2) The organometallic catalyst includes one or more of dibutyltin dilaurate, stannous octoate, lead isooctanoate, zinc bismuth composite catalyst, bismuth isooctanoate and zinc neodecanoate.

6. The two-component polyurethane sealant according to any one of claims 1-3, 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.

7. A method for preparing the two-component polyurethane sealant according to any one of claims 1-6, 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 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 in a mass ratio of (1~4):1 and then curing them.

8. The method according to claim 7, 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, plasticizer, filler and chain extender are mixed and heated to 80°C~120°C, and dehydrated under vacuum for 1h~5h until the water content drops to below 600ppm to obtain a premix. The premixed material is cooled to below 40°C, and the catalyst is added and mixed and stirred evenly under vacuum conditions.

9. The method according to claim 8, characterized in that, A first coupling agent is also added during the mixing process of the premix and the catalyst.

10. The method according to claim 7, characterized in that, The mixing process of the components contained in component B includes: The curing agent and colorant are mixed under vacuum conditions, and the thickener is added while stirring until the viscosity reaches (3 × 10⁻⁶). 4 )mPa∙s~(12×10 4 )mPa∙s.

11. The method according to claim 10, characterized in that, In the mixing step of adding the curing agent and the color paste, at least one of a second coupling agent, a catalyst, and a plasticizer is also added.

12. The method according to claim 10, 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 in the stirring state is 50r / min to 500r / min.

13. 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 1-6 or the two-component polyurethane sealant prepared by the method according to any one of claims 7-12.

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