Silane-modified polyether waterproof coating, its preparation method and use of modified epoxy resin

Abstract

The present application discloses a silane-modified polyether waterproof coating, its preparation method, and the use of a modified epoxy resin. The coating comprises components by weight: 100 parts by weight of a Wacker alkoxy-terminated polyether; 62 - 95 parts by weight of a Zhonghua alkoxy-terminated polyether; 40 - 80 parts by weight of a hydroxyl silicone oil; 230 - 350 parts by weight of an epoxy active plasticizer; 400 - 720 parts by weight of a pigment extender; 12 - 18 parts by weight of a modified epoxy resin containing terminal epoxy groups, alkoxysilyl groups, and epoxyalkyl acrylate monomer-derived segments; 4 - 21 parts by weight of a latent curing agent; 6 - 11 parts by weight of a water scavenger; 1 - 3 parts by weight of an accelerator; 1 - 2.5 parts by weight of a catalyst. The hydrolysis of the alkoxysilyl groups of the modified epoxy resin crosslinks with the alkoxy-terminated polyether, the hydroxyl silicone oil, and the hydroxyl groups on the substrate to enhance the adhesion. The modified epoxy resin and the hydroxyl silicone oil improve the adhesion and anti-peeling properties of the coil. The hydrolyzed latent curing agent reacts with the epoxy groups of the modified epoxy resin and the epoxy active plasticizer to prevent migration.

Description

Technical Field

[0001] This application belongs to the technical field of waterproof coatings, and particularly relates to a silane-modified polyether waterproof coating, a preparation method thereof, and the use of a modified epoxy resin. Background Art

[0002] Silane-modified polyether waterproof coating is a one-component, solvent-free waterproof coating prepared based on a modified polyether resin, with functional auxiliaries, fillers, and catalysts added. It has the advantages of high elongation, high tensile strength, good low-temperature flexibility, and low water absorption. Silane polyether resin, also known as end-silane modified polyether resin or organosilicon modified polyether resin, initially mainly appeared in the form of end-silyl polyether sealants. Silyl polyether sealants, also known as MS sealants, organosilicon modified polyether sealants, and modified silicone sealants, are applied on the base layer during use and cured by reacting with moisture to form a continuous and seamless high-molecular elastic waterproof film. Silane-modified polyether waterproof coating can be used for roofing, exterior walls, etc. under the condition of applying an appropriate protective layer. This coating can be constructed to the designed thickness in one pass by scraping, rolling, brushing, spraying, etc., saving time and construction costs.

[0003] In the field of building waterproofing, silane-modified polyether waterproof coating can be used to form a second waterproof layer in combination with some cold-applied waterproof membranes. A good bonding interface can be formed between the silane-modified polyether waterproof coating and the waterproof membrane surface, showing excellent bonding performance. The formed coating-membrane adhesive layer has excellent bonding and adhesion performance, the bonding layer is tight and impermeable, with excellent performance, overall excellent waterproof effect, and long service life, etc., and it has been promoted as a new type of waterproof coating. However, the inventors of this application found that during the use of silane-modified polyether waterproof coating, the traditional silane-modified polyether waterproof coating can cause compatibility problems with waterproof membranes due to the migration of plasticizers. The migration of plasticizers can cause a swelling effect on waterproof membranes, especially those composed of components such as asphalt and butyl rubber, reducing the cohesive force and adhesive peel performance of the membrane components to varying degrees. At the same time, the traditional silane-modified polyether waterproof coating has an unsatisfactory bonding effect on the cement base surface, with low bonding performance, and also has certain requirements for the dryness of the base surface. It is not easy to apply and construct on a concrete base surface with standing water. The coating has poor wettability, and the bonding strength drops significantly, resulting in a poor bonding effect, unable to meet the construction progress requirements and waterproof requirements. Therefore, how to prepare a silane-modified polyether waterproof coating with excellent bonding, no compatibility problems such as plasticizer migration with waterproof membranes, and capable of being directly constructed on a wet base surface has become an urgent problem to be solved currently. Summary of the Invention

[0004] The embodiments of the present application provide a silane-modified polyether waterproof coating and the silane-modified polyether waterproof coating prepared by its preparation method, which can be directly constructed on a wet concrete base surface, improve the adhesion performance and anti-peeling performance with waterproof coiled materials, and prevent the migration of plasticizers.

[0005] In a first aspect, the present application provides a silane-modified polyether waterproof coating, which comprises the following components calculated by weight: 100 parts by weight of Wacker alkoxy-terminated polyether; 62 - 95 parts by weight of Zhonghua alkoxy-terminated polyether; 40 - 80 parts by weight of hydroxy silicone oil; 230 - 350 parts by weight of epoxy active plasticizer; 400 - 720 parts by weight of pigment filler; 12 - 18 parts by weight of modified epoxy resin; the modified epoxy resin contains terminal epoxy groups, alkoxysilyl groups and epoxyalkyl acrylate monomer-derived segments; 4 - 21 parts by weight of latent curing agent; 6 - 11 parts by weight of water remover; 1 - 3 parts by weight of accelerator; 1 - 2.5 parts by weight of catalyst.

[0006] According to the embodiments of the first aspect of the present application, the epoxy equivalent of the modified epoxy resin is 260 g / mol - 430 g / mol.

[0007] According to the embodiments of the first aspect of the present application, the Wacker alkoxy-terminated polyether is selected from STP-E35, STP-E30, STP-E15, STP-E10 or a combination thereof.

[0008] According to the embodiments of the first aspect of the present application, the Zhonghua alkoxy-terminated polyether is selected from SAX227, SAX327, SAX220, SAX750 or a combination thereof.

[0009] According to the embodiments of the first aspect of the present application, the hydroxy silicone oil is selected from hydroxy-terminated polydimethylsiloxane with a viscosity of 350 cs - 750 cs or a combination thereof.

[0010] According to the embodiments of the first aspect of the present application, the epoxy active plasticizer is selected from epoxy soybean oil, epoxy linseed oil, epoxy cottonseed oil, epoxy rice bran oil, epoxy sunflower oil or a combination thereof.

[0011] According to the embodiments of the first aspect of the present application, the pigment filler is selected from fumed silica, nano calcium carbonate, heavy calcium, modified heavy calcium, nano kaolin, carbon black, modified kaolin or a combination thereof.

[0012] According to the embodiments of the first aspect of the present application, the modified epoxy resin comprises the structure shown in formula (3):

[0013]

[0014] In formula (3), n is an integer from 1 to 25, and R 1 is a straight-chain alkylene or branched-chain alkylene with no less than 2 carbon atoms, and R2 is an alkyl group having 1 to 3 carbon atoms, R 3 is a straight-chain or branched-chain alkyl group having 1 to 3 carbon atoms, and m 1 + m 2 = 3; R 4 includes groups having the following structural formulas:

[0015]

[0016] In formula (4), X is an integer from 1 to 3, R 5 is H, R 6 is an epoxyalkyl group having 3 or 7 carbon atoms, R 7 is H or methyl, represents the position where R 4 is connected to the molecular chain backbone of the modified epoxy resin.

[0017] According to an embodiment of the first aspect of the present application, the latent curing agent is selected from aldehyde imines, ketone imines, oxazolidines or combinations thereof.

[0018] According to an embodiment of the first aspect of the present application, the latent curing agent is selected from XY-401, YRLH-1106, JW505 or combinations thereof.

[0019] According to an embodiment of the first aspect of the present application, the water scavenger is selected from vinyltrimethoxysilane, vinyltriacetoxysilane, vinyltriethoxysilane or combinations thereof.

[0020] According to an embodiment of the first aspect of the present application, the promoter is selected from triacetoxyethylsilane, vinyltriacetoxysilane, diethyldiacetoxysilane or combinations thereof.

[0021] According to an embodiment of the first aspect of the present application, the catalyst is selected from dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, chelated tin catalysts or combinations thereof.

[0022] According to an embodiment of the first aspect of the present application, the chelated tin catalyst can be U-220H, WCAT-NS01, SG-U303.

[0023] Second aspect, the present application provides a preparation method of the above-mentioned silane-modified polyether waterproof coating, including: dispersing and treating Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxyl silicone oil, epoxy active plasticizer, pigments and fillers to obtain a second dispersion slurry; heating the second dispersion slurry to 100°C - 110°C and performing dehydration treatment under vacuum to obtain a dehydrated product; cooling the dehydrated product to 0°C - 70°C, adding the above-mentioned modified epoxy resin and latent curing agent and performing vacuum dispersion treatment to obtain a first modified product; cooling the first modified product to 50°C - 60°C, adding a water scavenger and a promoter and performing vacuum dispersion treatment to obtain a second modified product; adding a catalyst to the second modified product and performing vacuum dispersion treatment to obtain the silane-modified polyether waterproof coating.

[0024] According to an embodiment of the second aspect of the present application, the preparation method of the silane-modified polyether waterproof coating further includes: cooling the silane-modified polyether waterproof coating to ≤50°C and filling with nitrogen for protection.

[0025] Third aspect, an embodiment of the present application provides a use of a modified epoxy resin for preparing a silane-modified polyether waterproof coating, wherein the modified epoxy resin contains a terminal epoxy group, an alkoxysilyl group, and an epoxyalkyl acrylate monomer-derived chain segment.

[0026] The silane-modified polyether waterproof coating and its preparation method according to the embodiments of the present application use a self-made modified epoxy resin. The special molecular structure of the terminal epoxy group, alkoxysilyl group, and epoxyalkyl acrylate monomer-derived chain segment contained in the modified epoxy resin can improve the adhesion and anti-peeling performance to asphalt waterproofing membranes; at the same time, it can greatly improve the adhesion performance of the coating to the concrete base surface, especially the adhesion performance to a wet base surface. After the alkoxysilyl group in the modified epoxy resin molecule is hydrolyzed, it can undergo a condensation cross-linking reaction with alkoxy-terminated polyether and hydroxyl silicone oil, and at the same time, improve the adhesion force through the condensation reaction of the alkoxysilyl group with the hydroxyl group on the base surface. The introduction of the modified epoxy resin and hydroxyl silicone oil improves the adhesion, water resistance, heat resistance, weather resistance, and flexibility of the coating film. In addition, the epoxy group in the modified epoxy resin molecule and the epoxy group in the epoxy active plasticizer further undergo a cross-linking reaction with the hydrolyzed latent curing agent, giving full play to the excellent adhesion characteristics of epoxy resin, so that there are no free plasticizer molecules after the coating is cured, preventing plasticizer migration. Moreover, the silane-modified polyether waterproof coating according to the embodiments of the present application does not generate bubbles during the curing process, effectively reducing the influence of construction temperature and humidity on the coating. Detailed implementation manners

[0027] The features and exemplary embodiments of various aspects of the present application will be described in detail below. To make the objectives, technical solutions, and advantages of the present application clearer and more understandable, the present application will be further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only intended to explain the present application and not to limit the present application. For those skilled in the art, the present application can be implemented without some of these specific details. The following description of the embodiments is only to provide a better understanding of the present application by showing examples of the present application.

[0028] It should be noted that, in this document, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprising", "including" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "comprising..." does not exclude the presence of additional identical elements in the process, method, article or device comprising the said element.

[0029] To solve the problems of the prior art, an embodiment of the present application provides a silane-modified polyether waterproof coating and a preparation method thereof.

[0030] First, the silane-modified polyether waterproof coating provided by the embodiment of the present application will be introduced below.

[0031] In a first aspect, an embodiment of the present application provides a silane-modified polyether waterproof coating, comprising the following components calculated by weight parts: Wacker alkoxy-terminated polyether, 100 parts by weight; Zhonghua alkoxy-terminated polyether, 62 - 95 parts by weight; hydroxy silicone oil, 40 - 80 parts by weight; epoxy active plasticizer, 230 - 350 parts by weight; pigment and filler, 400 - 720 parts by weight; modified epoxy resin, 12 - 18 parts by weight; the modified epoxy resin contains terminal epoxy groups, alkoxysilyl groups and epoxyalkyl acrylate monomer-derived segments; latent curing agent, 4 - 21 parts by weight; water remover, 6 - 11 parts by weight; accelerator, 1 - 3 parts by weight; catalyst, 1 - 2.5 parts by weight.

[0032] The silane-modified polyether waterproof coating of the embodiment of the present application incorporates a self-made modified epoxy resin. The special molecular structure of the terminal epoxy group, alkoxysilyl group, and epoxyalkyl acrylate monomer-derived segment contained in the modified epoxy resin can enhance the adhesion and anti-peeling performance to the waterproof coiled material, and at the same time can greatly improve the adhesion performance to the concrete base surface, especially the wet base surface. After the alkoxysilyl group in the modified epoxy resin molecule is hydrolyzed, it can undergo a condensation cross-linking reaction with alkoxy-terminated polyether and hydroxy silicone oil, and at the same time improve the adhesion force through the condensation reaction with the hydroxyl group on the concrete base surface. The introduction of the modified epoxy resin and hydroxy silicone oil improves the adhesion, water resistance, heat resistance, weather resistance, and flexibility of the coating film. In addition, the epoxy groups in the modified epoxy resin molecule and the epoxy groups in the epoxy active plasticizer further undergo a cross-linking reaction with the hydrolyzed latent curing agent, giving full play to the excellent adhesion property of the epoxy resin. After curing, there are no free plasticizer molecules, preventing the migration of the plasticizer, and thus preventing the compatibility problems of the waterproof coiled material caused by its migration. Moreover, the silane-modified polyether waterproof coating of the embodiment of the present application does not generate bubbles during the curing process, effectively reducing the influence of the coating construction temperature and humidity on the coating.

[0033] In the embodiment of the present application, the molecular chain backbone of the modified epoxy resin has a terminal epoxy group, an alkoxysilyl group, and an epoxyalkyl acrylate monomer-derived segment. In each mole of the modified epoxy resin, since the addition amount of the ureido silane coupling agent is equal to or slightly greater than that of the bisphenol A type epoxy resin, the content of the alkoxysilyl group prepared correspondingly is equal to or slightly greater than that of the modified epoxy resin, and it may contain 1 mol to 3 mol of siloxanyl groups, that is, the substituents in the alkoxysilyl group may be 1 or 2 or 3 siloxanyl groups. Exemplarily, the content of the siloxanyl group in each mole of the modified epoxy resin may be 1.2 mol, 1.4 mol, 1.5 mol, 1.6 mol, 1.8 mol, 2.0 mol, 2.2 mol, 2.4 mol, 2.5 mol, 2.7 mol, 2.8 mol, 2.9 mol, 3.0 mol.

[0034] In some embodiments of the present application, the epoxy equivalent of the modified epoxy resin is 260 g / mol to 430 g / mol. The modified epoxy resin of the present application has a suitable epoxy equivalent range. Especially, the modified epoxy resin within the above epoxy equivalent range not only has high activity, fast cross-linking speed, and high cross-linking density, which can improve the peel strength and adhesion performance of the waterproof coiled material, but also can further take into account the heat resistance and mechanical strength of the coating, such as tensile strength, tear strength, etc. Exemplarily, the epoxy equivalent of the modified epoxy resin is 264 g / mol, 274 g / mol, 300 g / mol, 318 g / mol, 350 g / mol, 380 g / mol, 390 g / mol, 400 g / mol, 407 g / mol, 420 g / mol, 430 g / mol.

[0035] In some embodiments of the present application, the Wacker alkoxy-terminated polyether is selected from STP-E35, STP-E30, STP-E15, STP-E10 or a combination thereof.

[0036] In some embodiments of the present application, the Kaneka alkoxy-terminated polyether is selected from SAX227, SAX327, SAX220, SAX750 or a combination thereof.

[0037] In the embodiments of the present application, the Wacker silane-modified polyether and the Kaneka silane-modified polyether have the meanings well-known in the art. The Wacker silane-modified polyether may represent a silane-modified polyether produced by the Wacker Group or a silane-modified polyether produced according to the production process of Wacker. The Kaneka silane-modified polyether may represent a silane-modified polyether produced by Kaneka Corporation (Kaneka, Kaneka) of Japan or a silane-modified polyether produced according to the production process of Kaneka. The Kaneka silane-modified polyether is generally prepared by grafting a silane compound containing a hydrolyzable siloxane group onto both ends of a bifunctional polyether through a specific chemical reaction.

[0038] In some embodiments of the present application, the hydroxy silicone oil is selected from hydroxy-terminated polydimethylsiloxane with a viscosity of 350 cs to 750 cs or a combination thereof.

[0039] Exemplarily, the hydroxy silicone oil is selected from hydroxy-terminated polydimethylsiloxane with a viscosity of 350 cs, 400 cs, 420 cs, 450 cs, 500 cs, 550 cs, 600 cs, 630 cs, 660 cs, 700 cs, 720 cs or a combination thereof. In some other embodiments, the hydroxy silicone oil may be hydroxy-terminated polydimethylsiloxane with a viscosity of 360 cs to 480 cs, 450 cs to 560 cs, 490 cs to 640 cs, 540 cs to 750 cs.

[0040] In the embodiments of the present application, the hydroxy group in the hydroxy silicone oil can undergo a condensation crosslinking reaction with the group after hydrolysis of the alkoxysilyl group in the modified epoxy resin, improving the adhesion of the coating.

[0041] In some embodiments of the present application, the reactive plasticizer is selected from epoxy soybean oil, epoxy linseed oil, epoxy cottonseed oil, epoxy rice bran oil, epoxy sunflower oil or a combination thereof.

[0042] In the embodiments of the present application, the epoxy vegetable oil utilizes the excellent adhesion property of the epoxy resin. Through the epoxy group in its molecule, it can undergo a crosslinking reaction with the hydrolyzed latent curing agent, so that there are no free plasticizer molecules after the coating is cured, preventing the migration of the plasticizer, and thus preventing the problem of compatibility in asphalt waterproofing membranes.

[0043] In some embodiments of the present application, the pigment extender is selected from fumed silica, nano calcium carbonate, heavy calcium carbonate, modified heavy calcium carbonate, nano kaolin, carbon black, modified kaolin or a combination thereof.

[0044] In the embodiments of the present application, the macromolecules formed by the reaction of modified epoxy resin, hydroxyl silicone oil, epoxy active diluent, Wacker alkoxy-terminated polyether and Zhonghua alkoxy-terminated polyether are physically entangled with each other, which can enhance the flexibility of the paint film. Combining with the pigment extender can further enhance the heat resistance and weather resistance of the paint film.

[0045] In some embodiments of the present application, the modified epoxy resin includes the structure shown in formula (3):

[0046]

[0047] In formula (3), n is an integer from 1 to 25, and R 1 is a straight-chain or branched-chain alkylene group with no less than 2 carbon atoms, and R 2 is an alkyl group with 1 to 3 carbon atoms, and R 3 is a straight-chain or branched-chain alkyl group with 1 to 3 carbon atoms, and m 1 +m 2 =3; R 4 includes the group with the following structural formula:

[0048]

[0049] In formula (4), X is an integer from 1 to 3, R 5 is H, R 6 is an epoxy alkyl group with 3 or 7 carbon atoms, R 7 is H or methyl, represents the position where R 4 is connected to the molecular chain backbone of the modified epoxy resin.

[0050] In the embodiments of the present application, m 1 represents the number of alkyl groups, m 2 represents the number of alkoxy groups, m 1 +m 2 =3 indicates that at least one alkoxy group is connected to the silicon atom to which R 1 is connected.

[0051] In some embodiments of the present application, in the modified epoxy resin shown in formula (3), n is an integer from 1 to 2, R 1 is propylene, R 2 is methyl, and R 3 is methyl or ethyl.

[0052] In some embodiments of the present application, in formula (4), R 4It is the structure shown in any one of Formula (4-a) to Formula (4-d):

[0053]

[0054]

[0055] In Formula (4-a) to Formula (4-d), R 5 are all H, X is an integer from 1 to 3, represents the position where R 4 is connected to the molecular chain backbone of the modified epoxy resin.

[0056] In the embodiments of the present application, the modified epoxy resin is prepared through the following steps: Bisphenol A epoxy resin and ureido silane coupling agent are mixed for reaction to prepare reactant A; among them, the reaction structural formula (1) for preparing the modified epoxy resin from bisphenol A epoxy resin and ureido silane coupling agent is:

[0057]

[0058] In reaction formula (1), n is an integer from 1 to 25, R 1 is a straight-chain alkylene or branched-chain alkylene with no less than 2 carbon atoms, R 2 is an alkyl group of C1-C3, R3 is a straight-chain or branched-chain alkyl group of C1-C3, and m 1 +m 2 =3;

[0059] Under the protection of inert gas, acrylic epoxy alkyl ester monomer and initiator are added to reactant A to prepare the modified epoxy resin; among them, the reaction structural formula for preparing the modified epoxy resin from reactant A and acrylic epoxy alkyl ester monomer is:

[0060]

[0061]

[0062] In reaction formula (2), n is an integer from 1 to 25, X is an integer from 1 to 3; R 1 is a straight-chain alkylene or branched-chain alkylene with no less than 2 carbon atoms, R 2 is an alkyl group of C1-C3, R 3 is a straight-chain or branched-chain alkyl group of C1-C3, and m 1 +m 2 =3; R 6 is an epoxy alkyl group of C3 or C7, R 7 is H or methyl, R 4 includes the group with the following structural formula:

[0063]

[0064] In formula (4), X is an integer from 1 to 3, and R 5 is H, and R 6 is an epoxyalkyl group of C3 or C7, and R 7 is H or methyl, represents the position where R 4 is connected to the molecular chain backbone of the modified epoxy resin.

[0065] In the embodiments of the present application, the modified epoxy resin has a special molecular structure, that is, its molecular structure contains terminal epoxy groups, alkoxysilyl groups, and epoxyalkyl acrylate monomer-derived segments. Among them, after hydrolysis, the alkoxysilyl group can undergo a condensation cross-linking reaction with alkoxy-terminated polyether and hydroxyl silicone oil. At the same time, the adhesion of the coating is improved through the condensation reaction of the alkoxysilyl group with the hydroxyl groups on the substrate surface, so as to greatly improve the adhesion performance of the coating to the concrete substrate surface, especially the adhesion performance to the wet concrete substrate surface, thereby enhancing the adhesion and anti-peeling performance of the coating to the asphalt waterproofing membrane and the concrete substrate surface. At the same time, the introduced modified epoxy resin and hydroxyl silicone oil can undergo a cross-linking reaction to generate long molecular chains, improving the adhesion, water resistance, weather resistance, and flexibility of the coating film. The epoxy groups in the terminal epoxy groups of the modified epoxy resin and the epoxyalkyl acrylate monomer-derived segments, and the epoxy groups in the epoxy active plasticizer further undergo a cross-linking reaction with the hydrolyzed latent curing agent, while enhancing the adhesion performance and physical properties of the coating film, retaining the plasticizer molecules in the coating film structure and no longer migrating, thus solving the problem of plasticizer migration and the resulting compatibility problem of the asphalt waterproofing membrane.

[0066] In some embodiments of the present application, during the preparation of the modified epoxy resin, bisphenol A epoxy resin, ureido silane coupling agent, and epoxyalkyl acrylate monomer are added in a molar ratio of 1:(1 - 1.05):(1 - 3) respectively.

[0067] In some embodiments of the present application, the bisphenol A epoxy resin is selected from bisphenol A epoxy resin E44, bisphenol A epoxy resin E51, bisphenol A epoxy resin 128, or a combination thereof. At least the above-mentioned types of bisphenol A epoxy resin purchased from Baling Petrochemical can be selected. The bisphenol A epoxy resin has high strength and adhesion performance, as well as good chemical resistance, and can improve the adhesion performance, anti-peeling performance, and weather resistance of the coating.

[0068] In some embodiments of the present application, the ureido silane coupling agent is selected from γ-ureidopropyltrimethoxysilane, γ-ureidopropyltriethoxysilane, 3-(diisopropylureidopropyl)triethoxysilane, or a combination thereof.

[0069] In some embodiments of the present application, the initiator is selected from benzoyl peroxide (BPO), tert-butyl peroxybenzoate (TBPB), benzoyl peroxide, tert-amyl peroxy-2-ethylhexanoate, 1,1-bis(tert-amylperoxy)cyclohexane, or a combination thereof.

[0070] In some embodiments of the present application, the acrylic epoxy alkyl ester monomers are selected from glycidyl acrylate, glycidyl methacrylate, 3,4-epoxycyclohexylmethyl methacrylate, 3,4-epoxycyclohexyl acrylate, or a combination thereof.

[0071] In some embodiments of the present application, the molar ratio of reactant A to glycidyl acrylate, reactant A to glycidyl methacrylate, or reactant A to 3,4-epoxycyclohexylmethyl methacrylate, reactant A to 3,4-epoxycyclohexyl acrylate, or alternatively, the molar ratio of reactant A to a combination of glycidyl methacrylate and 3,4-epoxycyclohexylmethyl methacrylate can all be 1:(1 - 3). Exemplarily, the molar ratio of reactant A to the acrylic epoxy alkyl ester monomers is 1:1.2, 1:1.5, 1:1.6, 1:1.75, 1:2, 1:2.4, 1:2.7, 1:2.8, 1:2.9, 1:3.

[0072] In some embodiments of the present application, the inert gas is selected from helium, nitrogen, argon, or a combination thereof.

[0073] As an example, the preparation method of the modified epoxy resin includes:

[0074] S1. Put the calculated amount of dried bisphenol A epoxy resin E44 into a reactor, add a mixed solvent of n-butanol and N,N-dimethylformamide with a volume ratio of 1:1. The amount of the mixed solvent is 10 wt.% - 15 wt.% of the total mass of the reaction. Start stirring until bisphenol A epoxy resin E44 is completely dissolved, and control the temperature of the liquid material to be 45°C - 50°C to obtain a dispersion of bisphenol A epoxy resin E44.

[0075] S2. Drop the calculated amount of ureido silane coupling agent into the dispersion of bisphenol A epoxy resin E44 in the reactor, and react at a constant temperature for 2 hours - 3 hours under a nitrogen protection atmosphere to obtain reactant A.

[0076] S3. Under nitrogen protection, continue to stir reactant A to make the temperature of reactant A reach 80 °C to 85 °C; then add a calculated amount of glycidyl methacrylate and benzoyl peroxide to reactant A in the reactor. The addition amount of benzoyl peroxide is 0.3 wt.% to 0.5 wt.% of the total mass of this reaction; continue to stir and raise the temperature to 90 °C to 95 °C, and keep the temperature constant for reaction for 6 hours to 7 hours; then evacuate the product and perform vacuum distillation for 0.5 hours to 1 hour to obtain the modified epoxy resin. Among them, bisphenol A epoxy resin E44, ureido silane coupling agent, and glycidyl methacrylate are added according to a molar ratio of 1:(1 - 1.05):(1 - 3) respectively.

[0077] The synthesis route of the modified epoxy resin in the example is shown by the following reaction structural formulas (1) - (2). Reaction structural formula (1):

[0078]

[0079] Reaction structural formula (2):

[0080]

[0081]

[0082] In the above reaction structural formulas (1) - (2), n is an integer from 1 to 25, and X is an integer from 1 to 3; R 1 is a straight-chain or branched-chain alkyl group with no less than 2 carbon atoms, R 2 is an alkyl group of C1 - C3, R 3 is a straight-chain or branched-chain alkyl group of C1 - C3, and m 1 +m 2 = 3; R 4 includes groups with the following structural formulas:

[0083]

[0084] In formula (4 - b), X is an integer from 1 to 3, R 5 is H, represents the position where R 4 is connected to the molecular chain backbone of the modified epoxy resin.

[0085] It is understandable that replacing glycidyl methacrylate with 3,4-epoxycyclohexylmethyl methacrylate or glycidyl acrylate or 3,4-epoxycyclohexyl methacrylate, or replacing it with glycidyl methacrylate and 3,4-epoxycyclohexylmethyl methacrylate, or replacing it with glycidyl methacrylate and glycidyl acrylate, or replacing it with 3,4-epoxycyclohexylmethyl methacrylate and glycidyl acrylate can all result in similar reactions.

[0086] In some embodiments of the present application, the latent curing agent is selected from aldehyde imines, ketone imines, oxazolidines or combinations thereof.

[0087] In some embodiments of the present application, the latent curing agent is selected from XY-401, YRLH-1106, JW505 or combinations thereof.

[0088] In some embodiments of the present application, the water scavenger is selected from vinyltrimethoxysilane, vinyltriacetoxysilane, vinyltriethoxysilane or combinations thereof.

[0089] In some embodiments of the present application, the promoter is selected from triacetoxyethylsilane, vinyltriacetoxysilane, diethyldiacetoxysilane or combinations thereof.

[0090] In some embodiments of the present application, the catalyst is selected from dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, chelated tin catalysts or combinations thereof.

[0091] In some embodiments of the present application, the chelated tin catalyst can be U-220H, WCAT-NS01, SG-U303.

[0092] In a second aspect, the present application provides a method for preparing the above-mentioned silane-modified polyether waterproof coating, including: dispersing and treating Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxy silicone oil, epoxy active plasticizer, pigments and fillers to obtain a second dispersion slurry; heating the second dispersion slurry to 100°C to 110°C and performing dehydration treatment under vacuum to obtain a dehydrated product; cooling the dehydrated product to 0°C to 70°C, adding modified epoxy resin and latent curing agent and performing vacuum dispersion treatment to obtain a first modified product; cooling the first modified product to 50°C to 60°C, adding water scavenger and promoter and performing vacuum dispersion treatment to obtain a second modified product; adding catalyst to the second modified product and performing vacuum dispersion treatment to obtain the silane-modified polyether waterproof coating.

[0093] The preparation method of the silane-modified polyether waterproof coating according to the embodiments of the present application first disperses Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxyl silicone oil, epoxy active plasticizer, and pigments and fillers to obtain a second dispersion slurry with uniform dispersion of each substance. Then, by introducing a latent curing agent and a self-made modified epoxy resin, the special molecular structure in the modified epoxy resin can improve the adhesion and anti-peeling performance to the waterproof coil. Among them, after the alkoxysilyl group in the modified epoxy resin molecule is hydrolyzed, it can undergo a condensation cross-linking reaction with alkoxy-terminated polyether and hydroxyl silicone oil. The introduction of the modified epoxy resin and hydroxyl silicone oil improves the adhesion, water resistance, heat resistance, weather resistance, and flexibility of the coating film. At the same time, the adhesion force can be improved through the condensation reaction of the alkoxysilyl group with the hydroxyl group on the base surface, which can greatly improve the adhesion performance to the concrete base surface, especially the wet base surface.

[0094] In addition, the epoxy groups in the modified epoxy resin molecule and the epoxy groups in the epoxy plasticizer further cross-link with the hydrolyzed latent curing agent to fully exert the excellent adhesion characteristics of the epoxy resin. After curing, there are no free plasticizer molecules, preventing the migration of the plasticizer, and thus preventing the problem of the compatibility of the plasticizer migration to the waterproof coil. During the curing process of the silane-modified polyether waterproof coating according to the embodiments of the present application, no bubbles are generated, and it is hardly affected by the construction temperature and humidity.

[0095] In some embodiments of the present application, the preparation method of the silane-modified polyether waterproof coating further includes: cooling the silane-modified polyether waterproof coating to ≤50°C and filling it with nitrogen for protection.

[0096] In some embodiments of the present application, the dispersion treatment of Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxyl silicone oil, epoxy active plasticizer, and pigments and fillers includes: dispersing Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxyl silicone oil, and epoxy active plasticizer to obtain a first dispersion slurry; heating the first dispersion slurry to 90°C - 100°C and adding pigments and fillers for dispersion treatment to obtain a second dispersion slurry.

[0097] Exemplarily, the preparation method of the silane-modified polyether waterproof coating comprises: adding Wacker silane-modified polyether, Zhonghua silane-modified polyether, hydroxyl silicone oil, and active plasticizer into a reactor for dispersion treatment to obtain a first dispersion slurry; heating the first dispersion slurry to 90°C - 100°C and adding pigments and fillers for dispersion treatment to obtain a second dispersion slurry; heating the second dispersion slurry to 100°C - 110°C, evacuating to perform dehydration treatment for 3 - 4 hours to obtain a dehydrated product; cooling the dehydrated product to 60°C - 70°C, adding modified epoxy resin and latent curing agent, and performing vacuum dispersion treatment for 0.5 - 1 hour to obtain a first modified product; cooling the first modified product to 50°C - 60°C, adding water scavenger and accelerator, and performing vacuum dispersion treatment for 0.5 - 1 hour to obtain a second modified product; adding a catalyst to the second modified product and performing vacuum dispersion treatment for 0.5 - 1 hour, cooling the product to ≤50°C, filling with nitrogen for protection, and discharging to obtain the silane-modified polyether waterproof coating.

[0098] In a third aspect, an embodiment of the present application provides a use of the above-mentioned modified epoxy resin for preparing a silane-modified polyether waterproof coating, wherein the modified epoxy resin contains the above-mentioned terminal epoxy group, alkoxysilyl group, and epoxyalkyl acrylate monomer-derived segment.

[0099] Test part

[0100] The following are the models / brands of some raw material components used in the examples and comparative examples and their available sources. The raw material components not mentioned in the examples or comparative examples can be obtained through commercial channels: bisphenol A epoxy resin E44, purchased from Baling Petrochemical; Wacker silane-modified polyether: STP-E35, purchased from Wacker Chemie (China) Co., Ltd.; Zhonghua silane-modified polyether: SAX750, purchased from Zhonghua Trading (Shanghai) Co., Ltd.; catalyst: chelated tin SG-U303, purchased from Guangzhou Jianyi Chemical Import and Export Co., Ltd.; aldehyde imine type latent curing agent XY-401, purchased from Suzhou Xiangyuan New Materials Co., Ltd.; water scavenger, vinyltrimethoxysilane; accelerator, triethoxyethylsilane; ureido silane coupling agent, γ-ureidopropyltrimethoxysilane.

[0101] Preparation of modified epoxy resin

[0102] Preparation Example 1

[0103] The preparation method of modified epoxy resin 1 comprises:

[0104] S1. Put the calculated amount of dried bisphenol A epoxy resin E44 into a reactor, add a mixed solvent of n-butanol and N,N-dimethylformamide with a volume ratio of 1:1. The amount of the mixed solvent is 12 wt.% of the total mass of the reaction. Start stirring until bisphenol A epoxy resin E44 is completely dissolved, and control the temperature of the feed liquid at 45°C - 50°C to obtain a dispersion of bisphenol A epoxy resin E44.

[0105] S2. Drop the calculated amount of ureido silane coupling agent into the dispersion of bisphenol A epoxy resin E44 in the reactor, and react at a constant temperature for 3 hours under a nitrogen protection atmosphere to obtain reactant A.

[0106] S3. Continue to stir reactant A under nitrogen protection to make the temperature of reactant A 80°C - 85°C; add the calculated amount of glycidyl methacrylate and benzoyl peroxide to reactant A in the reactor. The addition amount of benzoyl peroxide is 0.3 wt.% of the total mass of the reaction; continue to stir and raise the temperature to 90°C - 95°C and react at a constant temperature for 6 hours; then evacuate the product and perform vacuum distillation for 1 hour to obtain modified epoxy resin 1. Among them, bisphenol A epoxy resin E44, ureido silane coupling agent and glycidyl methacrylate are added according to a molar ratio of 1:1.02:1 respectively, and the epoxy equivalent of modified epoxy resin 1 is 407 g / mol.

[0107] Preparation Example 2

[0108] The preparation method of modified epoxy resin 2 is only different from the preparation method of Preparation Example 1 in that: bisphenol A epoxy resin E44, ureido silane coupling agent and glycidyl methacrylate are added according to a molar ratio of 1:1.02:2 respectively, and the epoxy equivalent of the modified epoxy resin is 318 g / mol.

[0109] Preparation Example 3

[0110] The preparation method of modified epoxy resin 3 is only different from the preparation method of Preparation Example 1 in that: bisphenol A epoxy resin E44, ureido silane coupling agent and glycidyl methacrylate are added according to a molar ratio of 1:1.02:3 respectively, and the epoxy equivalent of the modified epoxy resin is 274 g / mol.

[0111] Preparation Example 4

[0112] The preparation method of modified epoxy resin 4 includes:

[0113] S1. Put the calculated amount of dried bisphenol A epoxy resin E44 into a reactor, add a mixed solvent of n-butanol and N,N-dimethylformamide with a volume ratio of 1:1. The amount of the mixed solvent used is 12 wt.% of the total mass of the reaction. Start stirring until bisphenol A epoxy resin E44 is completely dissolved, and control the temperature of the feed liquid to be 45°C - 50°C to obtain a dispersion of bisphenol A epoxy resin E44;

[0114] S2. According to the molar ratio of bisphenol A epoxy resin E44 to ureido silane coupling agent of 1:1.02, drop the calculated amount of ureido silane coupling agent into the dispersion of bisphenol A epoxy resin E44 in the reactor, and carry out a constant-temperature reaction for 3 hours under a nitrogen protection atmosphere to obtain modified epoxy resin 4. The epoxy equivalent of modified epoxy resin 4 is 672 g / mol.

[0115] Preparation Example 5

[0116] The preparation method of modified epoxy resin 5 includes:

[0117] S1. Put the calculated amount of dried bisphenol A epoxy resin E44 into a reactor, add a mixed solvent of n-butanol and N,N-dimethylformamide with a volume ratio of 1:1. The amount of the mixed solvent used is 12 wt.% of the total mass of the reaction. Start stirring until bisphenol A epoxy resin E44 is completely dissolved, and control the temperature of the feed liquid to be 45°C - 50°C to obtain a dispersion of bisphenol A epoxy resin E44;

[0118] S2. Continue to stir bisphenol A epoxy resin E44 under nitrogen protection to make the temperature of the feed liquid of bisphenol A epoxy resin E44 be 80°C - 85°C; then according to the molar ratio of bisphenol A epoxy resin E44 to glycidyl methacrylate of 1:1, add the calculated amount of glycidyl methacrylate and benzoyl peroxide into the dispersion of bisphenol A epoxy resin E44 in the reactor. The addition amount of benzoyl peroxide is 0.3 wt% of the total mass of the reaction. Continue to stir and raise the temperature to 90°C - 95°C, and carry out a constant-temperature reaction for 6 hours; then evacuate the product and carry out vacuum distillation for 1 hour to obtain modified epoxy resin 5. The epoxy equivalent of modified epoxy resin 5 is 197 g / mol.

[0119] Example 1

[0120] A silane-modified polyether waterproof coating, comprising the following components calculated by weight: Wacker alkoxy-terminated polyether is STP-E35, 100 parts by weight; Zhonghua alkoxy-terminated polyether is SAX750, 64 parts by weight; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750 cs), 52 parts by weight; active plasticizer is epoxy soybean oil, 280 parts by weight; pigment and filler, 590 parts by weight, including 360 parts by weight of heavy calcium carbonate and 230 parts by weight of nano calcium carbonate; modified epoxy resin 1, 13 parts by weight; the modified epoxy resin contains terminal epoxy groups, terminal silaneoxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, XY-401, 18 parts by weight; water scavenger is vinyltrimethoxysilane, 7 parts by weight; accelerator is triacetoxyethylsilane, 2 parts by weight; chelating tin catalyst SG-U303, 1.6 parts by weight.

[0121] The preparation method of the silane-modified polyether waterproof coating of this example includes: dispersing Wacker silane-modified polyether STP-E35, Zhonghua silane-modified polyether SAX750, hydroxy silicone oil hydroxy-terminated polydimethylsiloxane, and active plasticizer epoxy soybean oil to obtain a first dispersion slurry; heating the first dispersion slurry to 90°C - 100°C and adding heavy calcium carbonate and nano calcium carbonate as pigment and filler for dispersion treatment to obtain a second dispersion slurry; heating the second dispersion slurry to 100°C - 110°C, evacuating to perform dehydration treatment for 3 hours to obtain a dehydrated product; cooling the dehydrated product to 60°C - 70°C, adding modified epoxy resin and aldehyde imine type latent curing agent XY-401 for vacuum dispersion treatment for 0.5 hours to obtain a first modified product; cooling the first modified product to 50°C - 60°C, adding vinyltrimethoxysilane as a water scavenger and adding triacetoxyethylsilane as an accelerator for vacuum dispersion treatment for 0.5 hours to obtain a second modified product; adding chelating tin catalyst SG-U303 to the second modified product for vacuum dispersion treatment for 0.5 hours - 1 hour, cooling the product to 48°C, filling with nitrogen for protection, and discharging to obtain the silane-modified polyether waterproof coating.

[0122] Example 2

[0123] A silane-modified polyether waterproof coating, comprising the following components calculated by weight: Wacker alkoxy-terminated polyether is STP-E35, 100 parts by weight; Zhonghua alkoxy-terminated polyether is SAX750, 64 parts by weight; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750 cs), 52 parts by weight; active plasticizer is epoxy soybean oil, 300 parts by weight; pigment and filler, 590 parts by weight, including 360 parts by weight of heavy calcium and 230 parts by weight of nano calcium carbonate; modified epoxy resin 1, 13 parts by weight; the modified epoxy resin contains terminal epoxy groups, terminal silane oxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, XY-401, 18 parts by weight; water scavenger is vinyltrimethoxysilane, 7 parts by weight; accelerator is triacetoxyethylsilane, 2 parts by weight; chelating tin catalyst SG-U303, 1.6 parts by weight. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0124] Example 3

[0125] A silane-modified polyether waterproof coating, comprising the following components calculated by weight: Wacker alkoxy-terminated polyether is STP-E35, 100 parts by weight; Zhonghua alkoxy-terminated polyether is SAX750, 79 parts by weight; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750 cs), 62 parts by weight; active plasticizer is epoxy soybean oil, 270 parts by weight; pigment and filler, 590 parts by weight, including 360 parts by weight of heavy calcium and 230 parts by weight of nano calcium carbonate; modified epoxy resin 1, 15 parts by weight; the modified epoxy resin contains terminal epoxy groups, terminal silane oxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, is XY-401, 12 parts by weight; water scavenger is vinyltrimethoxysilane, 7 parts by weight; accelerator is triacetoxyethylsilane, 2.5 parts by weight; chelating tin catalyst SG-U303, 1.2 parts by weight. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0126] Example 4

[0127] A silane-modified polyether waterproof coating, comprising the following components calculated by weight: Wacker alkoxy-terminated polyether is STP-E35, 100 parts by weight; Zhonghua alkoxy-terminated polyether is SAX750, 64 parts by weight; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750 cs), 52 parts by weight; reactive plasticizer is epoxidized soybean oil, 280 parts by weight; pigment and filler, 590 parts by weight, including 360 parts by weight of heavy calcium and 230 parts by weight of nano calcium carbonate; modified epoxy resin 1, 15 parts by weight; the modified epoxy resin contains terminal epoxy groups, terminal silaneoxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, is XY-401, 18 parts by weight; water scavenger is vinyltrimethoxysilane, 7 parts by weight; accelerator is triacetoxyethylsilane, 2 parts by weight; chelating tin catalyst SG-U303, 1.6 parts by weight. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0128] Example 5

[0129] A silane-modified polyether waterproof coating, comprising the following components calculated by weight: Wacker alkoxy-terminated polyether is STP-E35, 100 parts by weight; Zhonghua alkoxy-terminated polyether is SAX750, 64 parts by weight; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750 cs), 52 parts by weight; reactive plasticizer is epoxidized soybean oil, 280 parts by weight; pigment and filler, 590 parts by weight, including 360 parts by weight of heavy calcium and 230 parts by weight of nano calcium carbonate; modified epoxy resin 1, 17 parts by weight; the modified epoxy resin contains terminal epoxy groups, terminal silaneoxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, is XY-401, 18 parts by weight; water scavenger is vinyltrimethoxysilane, 7 parts by weight; accelerator is triacetoxyethylsilane, 2 parts by weight; chelating tin catalyst SG-U303, 1.6 parts by weight. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0130] Example 6

[0131] A silane-modified polyether waterproof coating, comprising the following components calculated by weight parts: Wacker alkoxy-terminated polyether is STP-E35, 100 weight parts; Zhonghua alkoxy-terminated polyether is SAX750, 64 weight parts; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750cs), 52 weight parts; active plasticizer is epoxy soybean oil, 280 weight parts; pigment and filler, 590 weight parts, including 360 weight parts of heavy calcium and 230 weight parts of nano calcium carbonate; modified epoxy resin 2, 13 weight parts; the modified epoxy resin contains terminal epoxy groups, terminal silaneoxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, is XY-401, 18 weight parts; water remover is vinyltrimethoxysilane, 7 weight parts; accelerator is triacetoxyethylsilane, 2 weight parts; chelating tin catalyst SG-U303, 1.6 weight parts. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0132] Example 7

[0133] A silane-modified polyether waterproof coating, comprising the following components calculated by weight parts: Wacker alkoxy-terminated polyether is STP-E35, 100 weight parts; Zhonghua alkoxy-terminated polyether is SAX750, 64 weight parts; hydroxy silicone oil is hydroxy-terminated polydimethylsiloxane (750cs), 52 weight parts; active plasticizer is epoxy soybean oil, 280 weight parts; pigment and filler, 590 weight parts, including 360 weight parts of heavy calcium and 230 weight parts of nano calcium carbonate; modified epoxy resin 3, 13 weight parts; the modified epoxy resin contains terminal epoxy groups, terminal silaneoxy groups and epoxy acrylate monomer-derived segments; aldehyde imine latent curing agent, is XY-401, 18 weight parts; water remover is vinyltrimethoxysilane, 7 weight parts; accelerator is triacetoxyethylsilane, 2 weight parts; chelating tin catalyst SG-U303, 1.6 weight parts. The preparation method of the silane-modified polyether waterproof coating in this example is the same as that in Example 1.

[0134] Comparative Example 1

[0135] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that in Example 1 is that it does not contain the hydroxy-terminated polydimethylsiloxane (750cs) in Example 1, and the same weight portion of epoxy soybean oil is used instead.

[0136] Comparative Example 2

[0137] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that in Example 1 is that it does not contain the epoxy soybean oil in Example 1, and the same weight portion of the common plasticizer dibutyl phthalate is used instead.

[0138] Comparative Example 3

[0139] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that of Example 1 lies in that: it does not contain the modified epoxy resin in Example 1, and the same weight parts of an aldehyde-imide type latent curing agent are used instead.

[0140] Comparative Example 4

[0141] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that of Example 1 lies in that: it does not contain the hydroxyl-terminated polydimethylsiloxane (750 cs) and the modified epoxy resin in Example 1, and the same weight parts of epoxy soybean oil and an aldehyde-imide type latent curing agent are used respectively instead.

[0142] Comparative Example 5

[0143] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that of Example 1 lies in that: the modified epoxy resin 1 in Example 1 is replaced by modified epoxy resin 4.

[0144] Comparative Example 6

[0145] A silane-modified polyether waterproof coating, the difference in its composition and preparation process from that of Example 1 lies in that: the modified epoxy resin 1 in Example 1 is replaced by modified epoxy resin 5.

[0146] Performance test

[0147] Performance tests were carried out on the silane-modified polyether waterproof coatings prepared in Examples 1-7 and Comparative Examples 1-6. The test methods are as follows:

[0148] I. Test methods

[0149] 1. Performance test of the film of the silane-modified polyether waterproof coating

[0150] The performance test of the film of the silane-modified polyether waterproof coating was carried out with reference to JC / T 2435-2018.

[0151] 2. Test method for the peel strength compliance of asphalt waterproofing membranes

[0152] The silane-modified polyether waterproof coatings prepared in Examples 1-7 and Comparative Examples 1-6 were laminated with asphalt waterproofing membranes with release films (Keshun APF-3000), and the 180° peel strength was tested after lamination. Specifically, it includes:

[0153] (1) Preparation of test pieces

[0154] The silane-modified polyether waterproof coatings prepared in Examples 1-7 and Comparative Examples 1-6 were respectively applied by cold construction on concrete substrates with the specifications of 400mm*200mm*40mm, and the coating thickness was 1.5±0.2mm. After coating, within the coating adaptation period, the release film of the asphalt waterproof coiled material was torn off and laid and covered on the coating layer, and it was compacted and fully adhered so that the asphalt waterproof coiled material and the silane-modified polyether waterproof coating were in a fully adhered state. After curing for 168h, the asphalt waterproof coiled material was cut to obtain test pieces, and the preset size of the bonding surface was maintained at 70*50mm. The peel strength of the test pieces at 180° was measured.

[0155] (2) Test method

[0156] The cement mortar block surfaces in the test pieces corresponding to Examples 1-7 and Comparative Examples 1-6 were installed in the fixture at one end of the electronic tensile testing machine, and the unbonded surface of the asphalt waterproof coiled material cut in the test piece opposite to the bonding surface was bent 180° and clamped in the fixture at the other end of the electronic tensile testing machine. Pay attention to accurately positioning the test piece of the chuck part to ensure that the applied tensile force is evenly distributed on the width of the test piece. Start the detection equipment and set the tensile speed to 100mm / min.

[0157] 3. Bonding strength test on wet base surface

[0158] The bonding strength test of the silane-modified polyether waterproof coating on the wet base surface was carried out in accordance with the provisions of GB / T16777-2008.

[0159] Record the test results of the above performance tests in Table 1 below:

[0160]

[0161] In Table 1, the cohesive failure within the coating layer indicates that the interfacial adhesion force of the coating layer and the coiled material composite peeling is greater than the cohesive strength of the coating layer material itself, and the interfacial failure indicates that the interfacial adhesion force of the coating layer and the coiled material composite peeling is less than the cohesive strength of the coating layer material itself.

[0162] From the component ratios of the silane-modified polyether waterproof coatings in Examples 1-7 and Comparative Examples 1-6 and the test results in Table 1, it can be seen that:

[0163] In Examples 1-3, the silane-modified polyether waterproof coatings are more excellent in various performances such as bonding strength, bonding strength on wet base surface, composite peel strength with asphalt waterproof coiled material, and peel failure form. In Comparative Examples 1-6, the bonding performance and composite peel strength of the silane-modified polyether waterproof coatings are significantly lower than those of the silane-modified polyether waterproof coatings in Examples 1-3.

[0164] From the test data of the composite peel strength (N / mm) of the silane-modified polyether waterproof coatings and the rolls in Examples 1-3 and Comparative Examples 1-6, it can be clearly seen that the composite peel of the silane-modified polyether waterproof coatings and the rolls in Examples 1-3 are all cohesive failures within the coating layer with 100%, and for the composite peel of the silane-modified polyether waterproof coatings and the rolls in Comparative Examples 1-4, only 55% - 70% are cohesive failures within the coating layer and the rest are interfacial failures. The combined use of hydroxy-terminated polydimethylsiloxane, epoxy plasticizer and modified epoxy resin in Examples 1-3 improves the adhesion performance of the silane-modified polyether waterproof coating to the asphalt waterproof roll, and also improves the adhesion performance to the base surface, especially the wet base surface.

[0165] It can be seen from Example 1, Example 6 and Example 7 that as the molar ratio of bisphenol A epoxy resin and ureido silane coupling agent in the modified epoxy resin increases, the epoxy equivalent value of the modified epoxy resin gradually decreases, and the tensile properties, especially the adhesion properties of the silane-modified polyether waterproof coating gradually improve, and the peel strength of the composite with the roll also gradually increases. It can be seen from Example 1, Example 4 and Example 5 that increasing the dosage of the modified epoxy resin will cause a significant decrease in the elongation rate of the film of the silane-modified polyether waterproof coating, but it can be seen that the adhesion properties and the peel properties of the composite with the roll are significantly improved.

[0166] As described above, the above is only the specific implementation manner of the present application. Those skilled in the art can clearly understand that for the convenience and brevity of description, the specific working process described above can refer to the corresponding process in the foregoing method embodiments and will not be repeated here. It should be understood that the protection scope of the present application is not limited thereto. Any person skilled in the art within the technical scope disclosed in the present application can easily think of various equivalent modifications or substitutions, and these modifications or substitutions should all be covered within the protection scope of the present application.

Claims

1. A silane-modified polyether waterproof coating, characterized in that: The composition comprises the following components calculated by weight: Wacker alkoxy-terminated polyether, 100 parts by weight; 62 to 95 parts by weight of potassium hydroxide alkoxy terminated polyether; Hydroxy silicone oil, 40-80 parts by weight; Epoxy reactive plasticizer, 230-350 parts by weight; Pigments and fillers: 400-720 parts by weight; Latent curing agent, 4 to 21 parts by weight; Dewatering agent, 6 to 11 parts by weight; Accelerator, 1 to 3 parts by weight; Catalyst, 1 to 2.5 parts by weight; Modified epoxy resin, 12-18 parts by weight; the modified epoxy resin contains terminal epoxy groups, alkoxysilane groups and epoxyalkyl acrylate monomer derived segments; The modified epoxy resin comprises a structure shown in formula (3): In formula (3), n is an integer of 1 to 25; R1 is a straight chain alkylene group or a branched chain alkylene group having not less than 2 carbon atoms; R2 is a C1-C3 alkyl group; R3 is a C1-C3 straight chain or branched chain alkyl group; and m1+m2=3; R4 includes a group of the following structural formula: In formula (4), X is an integer of 1 to 3, R5 is H, R6 is a C3 or C7 alkylene oxide, R7 is H or methyl, It indicates the position where R4 is connected to the molecular chain backbone of the modified epoxy resin.

2. The silane-modified polyether waterproof coating according to claim 1, characterized in that: Meet any of the following requirements: 1) In formula (3), n is an integer of 1 to 2; R1 is a propylene group, R2 is a methyl group, and R3 is a methyl group or an ethyl group; 2) In formula (4), R4 is a structure represented by any one of formulas (4-a) to (4-d): In formulas (4-a) to (4-d), R5 is H, X is an integer of 1 to 3, It indicates the position where R4 is connected to the molecular chain backbone of the modified epoxy resin.

3. The silane-modified polyether waterproof coating according to claim 1 or 2, characterized in that: The modified epoxy resin is prepared by the following preparation steps: A bisphenol A epoxy resin and a urea-based silane coupling agent are mixed and reacted to prepare a reactant A; wherein the reaction structure (1) for preparing a modified epoxy resin by reacting the bisphenol A epoxy resin and the urea-based silane coupling agent is: In the reaction structure (1), n ​​is an integer of 1 to 25, R1 is a straight chain alkylene group or a branched chain alkylene group having not less than 2 carbon atoms, R2 is a C1-C3 alkyl group, R3 is a C1-C3 straight chain or branched chain alkyl group, and m1+m2=3; Under the protection of inert gas, an acrylate epoxy alkyl ester monomer and an initiator are added to the reactant A to prepare a modified epoxy resin; wherein the reaction formula (2) for preparing the modified epoxy resin from the reactant A and the acrylate epoxy alkyl ester monomer is: In the reaction structure (2), n is an integer of 1 to 25; R1 is a straight chain alkylene or branched chain alkylene having not less than 2 carbon atoms, R2 is a C1-C3 alkyl group, R3 is a C1-C3 straight chain or branched chain alkyl group, and m1+m2=3; R6 is a C3 or C7 alkylene oxide group, R7 is H or methyl, and R4 includes a group of the following structure: In formula (4), X is an integer of 1 to 3, R5 is H, R6 is a C3 or C7 alkylene oxide, R7 is H or methyl, It indicates the position where R4 is connected to the molecular chain backbone of the modified epoxy resin.

4. The silane-modified polyether waterproof coating according to claim 3, characterized in that: Meet at least one of the following requirements: The bisphenol A epoxy resin is selected from bisphenol A epoxy resin E44, bisphenol A epoxy resin E51, bisphenol A epoxy resin 128 or a combination thereof; The urea-based silane coupling agent is selected from γ-urea-based propyl trimethoxy silane, γ-urea-based propyl triethoxy silane, 3-(diisopropylurea-based propyl) triethoxy silane or a combination thereof; The initiator is selected from dibenzoyl peroxide, tert-butyl perbenzoate, benzoyl peroxide, tert-amyl peroxy-2-ethylhexyl ester, 1,1-bis(tert-amylperoxy)cyclohexane or a combination thereof; The bisphenol A epoxy resin, the urea-based silane coupling agent and the epoxyalkyl acrylate monomer are added in a molar ratio of 1: (1-1.05): (1-3); The epoxyalkyl acrylate monomer is selected from 2,3-epoxypropyl acrylate, glycidyl methacrylate, 3,4-epoxycyclohexyl methyl methacrylate, 3,4-epoxycyclohexyl methacrylate or a combination thereof.

5. The silane-modified polyether waterproof coating according to claim 1, characterized in that: Meet any of the following requirements: The epoxy equivalent of the modified epoxy resin is 260 g / mol to 430 g / mol; The Wacker alkoxy-terminated polyether is selected from STP-E35, STP-E30, STP-E15, STP-E10 or a combination thereof; The potassium alkoxy terminated polyether is selected from SAX227, SAX327, SAX220, SAX750 or a combination thereof; The hydroxy silicone oil is selected from hydroxyl-terminated polydimethylsiloxane with a viscosity of 350cs to 750cs; The epoxy reactive plasticizer is selected from epoxidized soybean oil, epoxidized linseed oil, epoxidized cottonseed oil, epoxidized rice bran oil, epoxidized sunflower oil or a combination thereof; The pigment filler is selected from fumed silica, nano calcium carbonate, heavy calcium carbonate, nano clay, carbon black, modified clay or a combination thereof; The latent curing agent is selected from aldimines, ketimines, oxazolidines or a combination thereof; The dewatering agent is selected from vinyl trimethoxy silane, vinyl triacetoxy silane, vinyl triethoxy silane or a combination thereof; The accelerator is selected from triacetoxyethylsilane, vinyl triacetoxysilane, diethyl diacetoxysilane or a combination thereof; The catalyst is selected from dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, chelated tin catalyst or a combination thereof.

6. The silane-modified polyether waterproof coating according to claim 5 meets any of the following requirements: The latent curing agent is selected from XY-401, YRLH-1106, JW505 or a combination thereof; The chelated tin catalyst is selected from U-220H, WCAT-NS01, SG-U303 or a combination thereof.

7. A method for preparing the silane-modified polyether waterproof coating according to any one of claims 1 to 6, characterized in that: include: Dispersing Wacker silane-modified polyether, silane-modified polyether, hydroxy silicone oil, epoxy active plasticizer, and pigments and fillers to prepare a second dispersed slurry; The second dispersed slurry is heated to 100° C. to 110° C. and vacuumed to perform dehydration treatment to obtain a dehydrated product; The dehydrated product is cooled to 60° C. to 70° C., and a modified epoxy resin and a latent curing agent are added to perform vacuum dispersion treatment to obtain a first modified product; The first modified product is cooled to 50° C. to 60° C., a dehydrating agent and an accelerator are added to perform vacuum dispersion treatment to obtain a second modified product; A catalyst is added to the second modified product for vacuum dispersion treatment to obtain a silane-modified polyether waterproof coating.

8. The preparation method according to claim 7, characterized in that: The Wacker silane-modified polyether, the silane-modified polyether, the hydroxy silicone oil, the epoxy active plasticizer, and the pigment and filler are dispersed and treated, including: Dispersing the Wacker silane-modified polyether, the potassium silane-modified polyether, the hydroxy silicone oil, and the epoxy reactive plasticizer to obtain a first dispersed slurry; The first dispersed slurry is heated to 90° C. to 100° C. and pigments and fillers are added for dispersion treatment to obtain a second dispersed slurry.

9. A use of a modified epoxy resin for preparing a silane-modified polyether waterproof coating, wherein: The modified epoxy resin contains terminal epoxy groups, alkoxysilane groups and epoxyalkyl acrylate monomer derived chain segments. The modified epoxy resin is a modified epoxy resin with a structure shown in formula (3) in claim 1.

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