Thixotropic agent for sealant, preparation method and application of thixotropic agent, epoxy sealant and preparation method of epoxy sealant
A thixotropic agent using polyamide wax and epoxy resin forms a three-dimensional network structure to address issues of gloss loss, odor, and debonding in epoxy caulking agents, improving stability and bonding strength.
Patent Information
- Application Number
- CN202411316244.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2024-12-20
AI Technical Summary
Epoxy caulking agents face issues such as the use of inferior curing agents causing gloss and color loss, phenolic substances leading to odor and health risks, and colloid debonding due to filler addition, failing to resist thermal expansion and contraction.
A thixotropic agent composed of polyamide wax, epoxy resin, and a diluent is introduced, forming a three-dimensional network structure with epoxy resin and gas silicone, enhancing bonding strength and reducing gas silicone use, while maintaining product stability and toughness.
The thixotropic agent improves storage stability, bonding strength, and reduces the risk of debonding, enhancing the product's environmental performance and construction durability.
Smart Images

Figure BDA0005052302290000051 
Figure BDA0005052302290000061 
Figure BDA0005052302290000062
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of seam beautifying agents, and more specifically, relates to a thixotropic agent for seam beautifying agents, a preparation method and application thereof, and an epoxy seam beautifying agent and a preparation method thereof. Background Art
[0002] In recent years, caulking agent has been valued and developed rapidly, and now has become an essential material in the field of decoration. From white cement in the past, to caulking agent later, to the current epoxy caulking agent, the product has been continuously upgraded, and has been greatly improved in terms of beauty, environmental protection and durability. However, as epoxy caulking agents are increasingly widely recognized and chosen by consumers, many manufacturers have gradually sacrificed product performance in pursuit of profits, resulting in various problems with epoxy caulking agents: (1) Selection of inferior curing agent raw materials - small molecule, highly volatile, highly corrosive basic amines. The introduction of this raw material can easily cause the caulking agent finished product to lose its gloss and color in a low temperature and high humidity environment, affecting consumers' pursuit of beauty and also accompanied by the risk of allergies; (2) Introduction of phenolic substances: In order to avoid the whitening phenomenon of the product in a low temperature and high humidity environment, a large amount of phenolic substances are introduced into the formula system to maintain the gloss of the product. However, the large amount of phenolic substances added can easily cause the product to have an excessive odor and, in severe cases, damage human health; (3) Colloid debonding and falling off: The addition of fillers causes the product's toughness to deteriorate, and it cannot meet the requirements of resisting deformation caused by thermal expansion and contraction of floor heating in northern winter. After construction, there is a risk of debonding and falling off of the base layer and the caulking agent. Summary of the invention
[0003] The purpose of the present invention is to provide a thixotropic agent for a seam beautifier, a preparation method and application thereof, and an epoxy seam beautifier and a preparation method thereof. The present invention develops a new type of thixotropic agent for a seam beautifier, thereby making the epoxy seam beautifier using the thixotropic agent less likely to absorb moisture and having good bonding strength, thereby solving the problem of easy debonding of the seam beautifier.
[0004] In order to achieve the above-mentioned object, a first aspect of the present invention provides a thixotropic agent for a seam beautifying agent. The raw materials for preparing the thixotropic agent for a seam beautifying agent include: polyamide wax, epoxy resin and a first diluent.
[0005] According to the present invention, preferably, in parts by weight, the amount of the polyamide wax is 8-20 parts, the amount of the epoxy resin is 10-25 parts, and the amount of the first diluent is 60-75 parts.
[0006] According to the present invention, preferably, the polyamide wax is D710 and / or AJK4560;
[0007] The epoxy resin is 128 epoxy resin and / or hydrogenated epoxy resin;
[0008] The first diluent is at least one of benzyl alcohol, AGE, 622 and 692.
[0009] In the present invention, the D710 is core chemical D710, and AJK4560 is Anjikang AJK4560.
[0010] The second aspect of the present invention provides a method for preparing the above-mentioned thixotropic agent for seam beautifying agent, the preparation method comprising: reacting the polyamide wax and epoxy resin in the presence of the first diluent, and removing unreacted reactants and the first diluent after the reaction to obtain the thixotropic agent for seam beautifying agent.
[0011] In the present invention, preferably, the preparation method comprises: (1) uniformly mixing the polyamide wax and a part of the first diluent to obtain a first dispersion; uniformly mixing the epoxy resin and the remaining first diluent to obtain a second dispersion; (2) contacting and reacting the second dispersion with the first dispersion, and removing the unreacted reactants and the first diluent after the reaction is completed to obtain the thixotropic agent for the seam beautifying agent.
[0012] According to the present invention, preferably, the reaction temperature is preferably 65-75°C.
[0013] In the present invention, preferably, the reaction time is 2.5-3.5h.
[0014] A third aspect of the present invention provides use of the thixotropic agent for a seam beautifying agent or the thixotropic agent for a seam beautifying agent prepared by the above preparation method in a seam beautifying agent.
[0015] A fourth aspect of the present invention provides an epoxy seam beautifying agent, the epoxy seam beautifying agent comprising component A and component B;
[0016] The component A comprises: epoxy resin, the thixotropic agent for the above-mentioned seam beautifying agent or the thixotropic agent for the seam beautifying agent prepared by the above-mentioned preparation method, a second diluent, a first thickener and an optional first defoaming agent;
[0017] The B component includes: a curing agent, a second thickener, a polyamide wax, a pigment and an optional second defoaming agent.
[0018] In the present invention, the introduction of a thixotropic agent for caulking agent into glue A can effectively reduce the proportion of gas silicone used in the caulking agent formula system (under the premise of ensuring the storage stability of the product for 12 months, the proportion of commercially available gas silicone glue A is greater than 5%, and the proportion of gas silicone in the present invention is less than 5%); the introduction of a polyamide wax thixotropic agent into glue B can effectively enhance the thixotropy of the caulking agent, build a spatial network structure, and improve the compactness of the product. Specifically, the introduction of a thixotropic agent for caulking agent can form a three-dimensional network structure with epoxy resin and gas silicone through hydrogen bonds, giving the product excellent thixotropy and compactness. At the same time, it is convenient to improve the degassing efficiency in the production process: the product destroys the network structure under high shear force, enhances fluidity, and facilitates degassing; and after the shear force is removed, the wax fiber structure is re-bridged to form a three-dimensional network structure again, giving the product excellent storage stability. The introduction of polyamide wax can effectively reduce the amount of gas silicone used, and can also effectively enhance the toughness and bonding effect of the finished caulking agent after curing.
[0019] In the present invention, the joint effect of the thixotropic agent for the caulking agent (glue A) and the polyamide wax thixotropic agent (glue B) can effectively enhance the compatibility effect of the caulking agent formula system, further improve the storage stability and bonding effect of the product; at the same time, with the aid of gas silicon and epoxy resin, the molecular structure forms intramolecular and intermolecular hydrogen bonds, maintains a spatial three-dimensional network structure, and greatly increases the thixotropic effect of the product.
[0020] According to the present invention, preferably, the component A comprises, by weight: 70-90 parts of epoxy resin, 1-10 parts of the thixotropic agent for the above-mentioned seam beautifying agent or the thixotropic agent for the seam beautifying agent prepared by the above-mentioned preparation method, 3-10 parts of the second diluent, 3-5 parts of the first thickener and 0-3 parts of the first defoaming agent;
[0021] In parts by weight, the B component includes: 70-90 parts of a curing agent, 3-5 parts of a second thickener, 5-10 parts of a polyamide wax, 1-10 parts of a pigment and 0-3 parts of a second defoaming agent.
[0022] In the present invention, in component B, the polyamide wax is preferably 5-7 parts by weight.
[0023] According to the present invention, preferably, the epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and hydrogenated epoxy resin;
[0024] The first thickener and the second thickener are each independently selected from hydrophilic silica and / or hydrophobic silica;
[0025] The second diluent is at least one of benzyl alcohol, C12-C14 alkyl glycidyl ether, phenyl glycidyl ether, butyl glycidyl ether and 1,4-butanediol glycidyl ether;
[0026] The polyamide wax is D710 and / or AJK4560;
[0027] The first defoamer and the second defoamer are each independently selected from at least one of BYK-1788, BYK-1610 and DF-110.
[0028] In the present invention, the pigment is selected from at least one of Kuncai, Guansheng and Beideli.
[0029] In the present invention, BYK-1788 and BYK-1610 were purchased from BYK Chemical Company; DF-110 was purchased from Momentive Company.
[0030] A fifth aspect of the present invention provides a method for preparing the above-mentioned epoxy seam beautifying agent, the preparation method comprising:
[0031] The epoxy resin, the thixotropic agent for the seam beautifying agent or the thixotropic agent for the seam beautifying agent prepared by the above preparation method, the second diluent, the first thickener and the optional first defoaming agent are stirred and mixed uniformly, and then vacuum defoamed to obtain the A component;
[0032] The curing agent, the second thickener, the polyamide wax, the pigment and the optional second defoaming agent are stirred and mixed uniformly, and then vacuum defoamed to obtain the B component.
[0033] In the present invention, preferably, in the preparation of component A, the stirring rate is 300-1000 r / min, and the time is 15-65 min; the vacuum degassing time is 20-30 min, and the vacuum degree is -0.08 MPa to -0.12 MPa;
[0034] In the preparation of component B, the stirring rate is 500-1000 r / min, and the time is 20-90 min; the vacuum degassing time is 20-30 min, and the vacuum degree is -0.08 MPa to -0.12 MPa.
[0035] The technical solution of the present invention has the following beneficial effects: the thixotropic agent for epoxy seam beautifier prepared by the present invention can significantly reduce the proportion of thickener gas silicon, enhance the environmental performance of the product, and effectively solve the construction problems such as the shedding of epoxy seam beautifier products.
[0036] Other features and advantages of the present invention will be described in detail in the following detailed description. DETAILED DESCRIPTION
[0037] The preferred embodiments of the present invention will be described in more detail below. Although the preferred embodiments of the present invention are described below, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided to make the present invention more thorough and complete, and to fully convey the scope of the present invention to those skilled in the art.
[0038] The present invention is further described below by examples:
[0039] In the following embodiments and comparative examples:
[0040] The polyamide wax used was selected from Core Chemical D710;
[0041] DF-110 is Maitu DF-110;
[0042] The curing agent used is prepared by the following method: (1) Mix the amino-terminated polyether and isophorone diamine in the formula, stir evenly and then slowly drop 10 parts of hydrogenated epoxy resin, control the reaction temperature not higher than 70°C, and keep warm at 75°C for 2 hours after the hydrogenated epoxy resin is added; (2) Add the 1,3-cyclohexanedimethylamine in the formula at one time, stir for 8 minutes, slowly drop the remaining hydrogenated epoxy resin, and keep warm at 75°C for 1 hour after the hydrogenated epoxy resin is added; (3) Slowly drop the active diluent and dispersant in the formula, keep warm at 75°C for 2 hours after the addition is completed, then add the accelerator in the formula at one time, stir for 8 minutes, evacuate for 25 minutes, control the vacuum degree at -0.1MPa, and cool to room temperature to obtain the curing agent. The specific formula of the curing agent is as shown in the following table. In the table, the amino-terminated polyether is Huntsman D220; the isophorone diamine is Evonik 1,3-Cyclohexyldimethylamine was from Mitsubishi of Japan; K-54 was from Evonik Ancamine; AGE was purchased from Green Home; hydrogenated epoxy resin was from Japan Idec hydrogenated epoxy resin 4080E; polycarboxylate ammonium salt was purchased from Japan Nopco SN5027.
[0043] Table 1
[0044]
[0045]
[0046] The thixotropic agent for the seam beautifying agent used is prepared by the following method: by weight, 10 parts of core chemical D710 (polyamide wax) are dissolved in 35 parts of benzyl alcohol, and after uniform dispersion, a first dispersion is obtained; at 70°C, a mixture consisting of 20 parts of epoxy resin and 35 parts of benzyl alcohol is slowly dripped into the first dispersion, and after the dripping is completed, the reaction is controlled at 70°C and the temperature is kept constant for 3 hours. After the reaction is completed, the unreacted raw materials (core chemical D710 and epoxy resin) and the first diluent benzyl alcohol are removed by reduced pressure distillation to obtain the thixotropic agent for the seam beautifying agent. Wherein, the epoxy resin is 128 epoxy resin.
[0047] Example 1
[0048] This embodiment provides an epoxy seam beautifying agent, which includes component A and component B, and the specific formula is as follows:
[0049] Table 2
[0050]
[0051]
[0052] The preparation method of the above-mentioned epoxy seam beautifying agent comprises the following steps:
[0053] S1: Add epoxy resin, the first thickener and the second diluent to a stirring kettle at room temperature, stir at 500 r / min for 20 min, then add the thixotropic agent for the seam beautifying agent and the first defoaming agent, stir at 1000 r / min for 30 min, vacuum degassing for 30 min, control the vacuum degree at -0.1 MPa, and pack the material to obtain component A, pack it into a seam beautifying agent hose, and seal it for storage;
[0054] S2: Add curing agent and second thickener to the stirring kettle at room temperature, stir at 500r / min for 20min, then add pigment, polyamide wax and second defoamer, stir at 1000r / min for 30min; vacuum degassing for 30min, control the vacuum degree at -0.1MPa, divide the material into components B, load them into the seam agent hose, and seal them for storage.
[0055] Example 2
[0056] This embodiment provides an epoxy seam beautifying agent, which includes component A and component B, and the specific formula is as follows:
[0057] Table 3
[0058]
[0059]
[0060] The preparation method of the epoxy sealant of this embodiment is the same as that of Example 1.
[0061] Example 3
[0062] This embodiment provides an epoxy seam beautifying agent, which includes component A and component B, and the specific formula is as follows:
[0063] Table 4
[0064]
[0065] The preparation method of the epoxy sealant of this embodiment is the same as that of Example 1.
[0066] Comparative Example 1
[0067] This comparative example provides an epoxy seam beautifying agent, which includes component A and component B, and the specific formula is as follows:
[0068] Table 5
[0069]
[0070] The preparation method of the above-mentioned epoxy seam beautifying agent comprises the following steps:
[0071] S1: Add epoxy resin, the first thickener and the second diluent to a stirring kettle at room temperature, stir at 500 r / min for 20 min, then add the first defoamer and stir at 1000 r / min for 30 min, vacuum degassing for 30 min, and control the vacuum degree at -0.1 MPa. Discharge the material in batches to obtain component A, load it into a seam sealant hose, and seal it for storage;
[0072] S2: Add curing agent and second thickener to the stirring kettle at room temperature, stir at 500r / min for 20min, then add pigment, polyamide wax and second defoamer, stir at 1000r / min for 30min; vacuum degassing for 30min, control the vacuum degree at -0.1MPa, divide the material into components B, load them into the seam agent hose, and seal them for storage.
[0073] Comparative Example 2
[0074] This comparative example provides an epoxy seam beautifying agent, which is Nippon Paint Qiaoyishi.
[0075] Test Case
[0076] The epoxy caulking agent of the above embodiment and comparative example was tested for the shoveling time, shoveling performance, hardness, bonding strength, abrasion resistance, flexural strength, compressive strength, shrinkage value, water absorption, VOC, and storage stability. The test results are shown in Table 5; wherein the hardness was tested according to GB / T 2411, the bonding strength was tested according to GB / T5210-2006, the abrasion resistance, flexural strength, compressive strength, shrinkage value, and water absorption were all tested according to JC / T 1004-2017, and VOC was tested according to GB18583;
[0077] Table 6
[0078]
[0079]
[0080] 1. From the data in Table 6 above, it can be seen that the introduction of the thixotropic agent for the seam beautifying agent in the present invention can significantly reduce the VOC of the seam beautifying agent product and prolong the storage stability of the product.
[0081] 2. From the data in Table 6 above, it can be seen that the combination of the thixotropic agent for the above-mentioned caulking agent and the polyamide wax can improve the curing rate of the caulking agent, and the hardness, wear resistance, compressive and flexural strength, shrinkage rate, water absorption and other parameters of the cured product are significantly better than those of the commercially available caulking agent. This shows that the introduction of the thixotropic agent for the above-mentioned caulking agent can effectively enhance the strength and various application properties of the caulking agent product.
[0082] 3. From the data in Table 6 above, it can be seen that the thixotropic agent for the above-mentioned caulking agent can effectively enhance the bonding strength of the caulking agent product, effectively solve the risk of the caulking agent falling off during the construction process, and give the product an excellent service life.
[0083] The embodiments of the present invention have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments.
Claims
1. A thixotropic agent for a seam beautifying agent, characterized in that: The raw materials for preparing the thixotropic agent for the seam beautifying agent include: polyamide wax, epoxy resin and a first diluent.
2. The thixotropic agent for a seam beautifying agent according to claim 1, wherein: In parts by weight, the polyamide wax is used in an amount of 8-20 parts, the epoxy resin is used in an amount of 10-25 parts, and the first diluent is used in an amount of 60-75 parts.
3. The thixotropic agent for a seam-beautifying agent according to claim 1 or 2, wherein: The polyamide wax is D710 and / or AJK4560; The epoxy resin is 128 epoxy resin and / or hydrogenated epoxy resin; The first diluent is at least one of benzyl alcohol, AGE, 622 and 692.
4. The method for preparing the thixotropic agent for seam beautifying agent according to any one of claims 1 to 3, characterized in that: The preparation method comprises: reacting the polyamide wax and epoxy resin in the presence of the first diluent, removing unreacted reactants and the first diluent after the reaction is completed, and obtaining the thixotropic agent for the seam beautifying agent.
5. The preparation method according to claim 4, wherein The temperature of the reaction is preferably 65-75°C.
6. Use of the thixotropic agent for seam beautifying agent according to any one of claims 1 to 3 or the thixotropic agent for seam beautifying agent prepared by the preparation method according to claim 4 or 5 in seam beautifying agent.
7. An epoxy seam beautifying agent, characterized in that: The epoxy seam beautifying agent comprises component A and component B; The component A comprises: epoxy resin, the thixotropic agent for seam beautifying agent according to any one of claims 1 to 3 or the thixotropic agent for seam beautifying agent prepared by the preparation method according to claim 4 or 5, a second diluent, a first thickener and an optional first defoaming agent; The B component includes: a curing agent, a second thickener, a polyamide wax, a pigment and an optional second defoaming agent.
8. The epoxy seam sealant according to claim 7, wherein: In parts by weight, the component A comprises: 70-90 parts of epoxy resin, 1-10 parts of the thixotropic agent for seam beautifying agent according to any one of claims 1-3 or the thixotropic agent for seam beautifying agent prepared by the preparation method according to claim 4 or 5, 3-10 parts of the second diluent, 3-5 parts of the first thickener and 0-3 parts of the first defoaming agent; In parts by weight, the B component includes: 70-90 parts of a curing agent, 3-5 parts of a second thickener, 5-10 parts of a polyamide wax, 1-10 parts of a pigment and 0-3 parts of a second defoaming agent.
9. The epoxy seam sealant according to claim 7 or 8, wherein: The epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and hydrogenated epoxy resin; The first thickener and the second thickener are each independently selected from hydrophilic silica and / or hydrophobic silica; The second diluent is at least one of benzyl alcohol, C12-C14 alkyl glycidyl ether, phenyl glycidyl ether, butyl glycidyl ether and 1,4-butanediol glycidyl ether; The polyamide wax is D710 and / or AJK4560; The first defoamer and the second defoamer are each independently selected from at least one of BYK-1788, BYK-1610 and DF-110.
10. The method for preparing the epoxy seam beautifying agent according to any one of claims 7 to 9, characterized in that: The preparation method comprises: The epoxy resin, the thixotropic agent for a seam beautifying agent according to any one of claims 1 to 3 or the thixotropic agent for a seam beautifying agent prepared by the preparation method according to claim 4 or 5, the second diluent, the first thickener and the optional first defoaming agent are stirred and mixed uniformly, and then vacuum defoamed to obtain the A component; The curing agent, the second thickener, the polyamide wax, the pigment and the optional second defoaming agent are stirred and mixed uniformly, and then vacuum defoamed to obtain the B component.
