Silane modified polyether sealant for indoor doors and windows and preparation method of silane modified polyether sealant

Abstract

The invention relates to a silane modified polyether sealant for indoor doors and windows and a preparation method of the silane modified polyether sealant. The silane modified polyether sealant comprises the following components: a silane modified polyether polymer, a plasticizer, a modified filler, an antioxidant, high-concentration silane master batch, a strengthening accelerant and the like. According to the silane modified polyether sealant, under the synergistic effect of the high-concentration master batch, the modified filler and the strengthening accelerant, the silane modified polyether sealant has the advantages of good storage stability, excellent weather resistance, high strengthening speed, high bonding force, capability of realizing rapid positioning, convenience in use, simple preparation method, low production cost and high practicability. And the method is suitable for industrial large-scale production.

Description

Technical Field

[0001] The invention belongs to sealants for building materials and home decoration, and in particular, relates to a silane-modified polyether sealant for indoor doors and windows and a preparation method thereof. Background Art

[0002] Silane modified polyether sealant combines the advantages of polyurethane sealant and silicone sealant, overcomes the shortcomings of both, has good mechanical properties, good coating, weather resistance, adhesion, and good stain resistance. Industrialized housing adopts the advantage of solvent-free, does not contain isocyanate, meets the European R-40 mandatory labeling, and has low VOC that can reach the highest European EC-1R standard. Therefore, most home improvement projects in Europe, the United States, Japan and other countries use silane modified polyether sealant for bonding, and it has low volatility, which is in line with the development trend of today's social environmental protection concept.

[0003] There are many technologies for public research on this type of sealant. CN 201810883371.7 discloses a method for preparing a silane-modified polyether sealant. It describes that when preparing silane-modified polyether sealants using existing processes, high-temperature dehydration treatment is used to reduce the water content in the reaction system and ensure the quality of the sealant products. However, high-temperature dehydration is prone to cause the inactivation of some raw materials, which greatly restricts the selection of raw materials. The product is easy to deteriorate, which is not conducive to long-term storage of the product. A method for preparing a silane-modified polyether sealant by pretreating the raw materials and controlling the reaction temperature is proposed to extend the shelf life of the sealant. However, since the pretreatment time of the raw materials is as high as 40 to 60 hours, the production and preparation process environment requirements are strict and complex, and it is not suitable for the production of industrialized building materials. CN 201810292582.3 discloses a high elasticity low modulus single-component silane modified polyether sealant and a preparation method thereof, by adding a small molecule silane coupling agent, equipped with a low-activity bismuth-based catalyst, and using a distributed reaction method, a low modulus silane modified polyether sealant with excellent tensile strength and good ductility is prepared. However, bismuth-based catalysts are mainly used in the fields of polyurethane coatings, polyurethane leather, polyurethane adhesives, polyurethane silicone rubber, PU resin slurry, etc., and due to their low activity, if they are not properly controlled, it is easy to cause the colloid to have a fast surface drying time, which is inconvenient for actual construction; the curing speed is slow, the strengthening time is long, and there is a risk of substrate bonding falling off. Summary of the invention

[0004] The purpose of the present invention is to overcome the shortcomings of the above-mentioned background technology and optimize these defects through the selection and modification of materials.

[0005] A silane-modified polyether sealant for indoor doors and windows, characterized in that it comprises the following raw materials in parts by weight: Silane modified polyether polymer 26-40 parts Plasticizer 20-30 parts Modified filler 30-40 parts Brightener 2-5 parts Antioxidant 0.1~1 part 1 to 3 parts of strengthening accelerator High concentration silane masterbatch 3-6 parts 1 to 3 parts of dewatering agent Catalyst 0.1~0.5 parts The silane-modified polyether polymer is one or more of the Kashima models SAX015, SAX303H and SAX750.

[0006] Furthermore, the plasticizer is a mixture of one or both of phthalates and polyether polyols. Furthermore, the modified filler is prepared by adding methylchlorosilane to the powder step by step, stirring and reacting at 150-180°C for 8-12 hours, then stirring for 3-5 hours under vacuum and constant temperature conditions, discharging the material after the reaction is completed, and grinding to obtain the modified filler.

[0007] The methylchlorosilane is further described as dimethyldichlorosilane; and the powder is calcium carbonate.

[0008] Furthermore, the whitening agent is needle-type titanium dioxide.

[0009] Furthermore, the antioxidant is specifically a mixture of one or more of 1076, 168, and 1010.

[0010] Furthermore, the strengthening accelerator is rosin resin or terpene resin.

[0011] Furthermore, the high-concentration silane masterbatch is prepared by adding the silane coupling agent to paraffin step by step, stirring and reacting at 80-120°C for 1-2 hours, stirring for 15-30 minutes under vacuum and constant temperature conditions, and after the reaction is completed, cooling to room temperature and grinding to obtain the high-concentration silane masterbatch.

[0012] Furthermore, the silane coupling agent is a mixture of one or more of γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, and N-aminoethyl-γ-aminopropyltriethoxysilane; the silane coupling agent is mixed and added in equal proportions, and the amount of the silane coupling agent added is 5 to 10%.

[0013] Furthermore, the dehydrating agent is a mixture of one or more of γ-mercaptopropyltrimethoxysilane, vinyltrimethoxysilane and methyltrimethoxysilane.

[0014] Furthermore, the catalyst is a mixture of one or more of stannous octoate, dibutyltin dilaurate, dibutyltin diacetate and dibutyltin diacetylacetonate.

[0015] The present invention also provides a method for preparing the above-mentioned silane-modified polyether sealant for indoor doors and windows, comprising the following steps: Weigh each raw material component according to the corresponding weight parts; (1) mixing the silane-modified polyether polymer, the plasticizer, the modified filler, the brightener, and the antioxidant uniformly; (2) Add a strong accelerator, stir and dehydrate for 1 hour under the conditions of vacuum degree 0.09MPa ~ 0.1MPa and temperature 100℃ ~ 120℃; (3) adding high concentration silane masterbatch and stirring for 0.5 h under the conditions of vacuum degree of 0.09 MPa to 0.1 MPa and temperature of 50°C to 80°C; (4) After cooling to below 50° C., a dehydrating agent and a catalyst are added, and the mixture is stirred under vacuum for 0.5 h to obtain the silane-modified polyether sealant.

[0016] The present invention adopts a self-made modified filler, and the moisture content of the powder is well reduced through spontaneous reaction. After high-temperature dehydration reaction, the surface of the powder is covered with some siloxane substances. In the later preparation process, the addition of a strong accelerator can greatly increase the curing depth of the colloid; and through the overall mixing method, the silane coupling agent is dispersed in paraffin in advance to prepare a masterbatch containing high-concentration silane, which can replace pure silane to well improve the dispersibility of the silane coupling agent in the silane-modified polyether polymer and the modified filler, and enhance the bonding strength of the colloid.

[0017] The present invention has the following technical effects: Provides a silane-modified polyether sealant for indoor doors and windows, which has the characteristics of good storage stability, excellent weather resistance, fast strengthening speed and high adhesion, and can achieve rapid positioning; Provided is a silane-modified polyether sealant for indoor doors and windows, which has the characteristics of simple preparation method, low production cost and applicability to industrial large-scale production. DETAILED DESCRIPTION

[0018] The following examples illustrate the present invention, but the present invention is not limited to these examples. Modifications to the specific embodiments of the present invention or equivalent replacement of some technical features without departing from the spirit of the present invention should be included in the scope of the technical solution claimed by the present invention.

[0019] Example 1 A silane-modified polyether sealant for indoor doors and windows, comprising the following raw materials and weight proportions: 26 parts of silane-modified polyether polymer SAX303H, 20 parts of polyether polyol PPG3000 as a plasticizer, 40 parts of modified fillers, 5 parts of titanium dioxide as a brightener, 0.2 parts of 1076 and 0.3 parts of 168 as antioxidants, 1 part of rosin resin and 1 part of terpene resin as strengthening accelerators, 4 parts of high-concentration silane masterbatch prepared from 5% γ-aminopropyltriethoxysilane, 2 parts of vinyltrimethoxysilane as a water remover, and 0.1 part of dibutyltin diacetylacetonate as a catalyst.

[0020] The preparation method of the silane-modified polyether sealant for indoor doors and windows comprises the following steps: After SAX303H, polyether polyol PPG3000, modified filler, titanium dioxide, 1076 and 168 are evenly mixed, rosin resin and terpene resin are added under vacuum degree of 0.09-0.1Mpa and temperature of 1001-120°C, and the mixture is stirred and dehydrated for 1 hour. The temperature is then cooled to 50-80°C, and high-concentration silane masterbatch prepared by γ-aminopropyltriethoxysilane is added under vacuum degree of 0.09-0.1Mpa. After high-speed stirring for 0.5h, the temperature is lowered to below 50°C, vinyltrimethoxysilane and dibutyltin dilaurate are added, and the mixture is stirred for 0.5h under vacuum to discharge the material.

[0021] Example 2 A silane-modified polyether sealant for indoor doors and windows, comprising the following raw materials and weight proportions: 30 parts of silane-modified polyether polymers SAX750 and SAX015, 10 parts of plasticizer DIDP, 35 parts of modified fillers, 2 parts of titanium dioxide as a whitening agent, 1 part of antioxidant 1010, 2 parts of terpene resin as a strengthening accelerator, 3 parts of high-concentration silane masterbatch prepared from a mixture of 9% γ-aminopropyltrimethoxysilane and N-aminoethyl-γ-aminopropyltriethoxysilane, 3 parts of dehydrating agent γ-mercaptopropyltrimethoxysilane, and 0.5 parts of dibutyltin dilaurate. The preparation method of the silane-modified polyether sealant for indoor doors and windows comprises the following steps: After SAX750, SAX015, DIDP, modified filler, titanium dioxide and 1010 are evenly mixed, terpene resin is added under vacuum degree of 0.09-0.1Mpa and temperature of 1001-120°C, and the mixture is stirred and dehydrated for 1h. The temperature is cooled to 50-80°C, and high-concentration silane masterbatch prepared by a mixture of γ-aminopropyltrimethoxysilane and N-aminoethyl-γ-aminopropyltriethoxysilane is added under vacuum degree of 0.09-0.1Mpa. After high-speed stirring for 0.5h, the temperature is lowered to below 50°C, γ-mercaptopropyltrimethoxysilane and dibutyltin dilaurate are added, and the mixture is stirred for 0.5h under vacuum to discharge the material.

[0022] Example 3 A silane-modified polyether sealant for indoor doors and windows, comprising the following raw materials and weight proportions: 35 parts of silane-modified polyether polymer SAX750, 25 parts of plasticizer DINP, 32 parts of modified filler, 3 parts of whitening agent titanium dioxide, 0.5 parts of antioxidants 168 and 0.5 parts of 1010, 1 part of strengthening accelerator terpene resin, 6 parts of high-concentration silane masterbatch prepared from 6.5% γ-aminopropyltrimethoxysilane, 1 part of dehydrating agent γ-mercaptopropyltrimethoxysilane and 0.5 parts of vinyltrimethoxysilane, and 0.2 parts of catalysts stannous octoate and 0.1 parts of dibutyltin diacetate.

[0023] The preparation method of the silane-modified polyether sealant for indoor doors and windows comprises the following steps: After SAX750, DINP, modified filler, titanium dioxide, 168 and 1010 are evenly mixed, terpene resin is added and stirred for dehydration for 1 hour under the conditions of vacuum degree of 0.09-0.1Mpa and temperature of 1001-120°C, the temperature is cooled to 50-80°C, high-concentration silane masterbatch prepared by γ-aminopropyltrimethoxysilane is added under the conditions of vacuum degree of 0.09-0.1Mpa, high-speed stirring is performed for 0.5h, the temperature is lowered to below 50°C, γ-mercaptopropyltrimethoxysilane, vinyltrimethoxysilane, stannous octoate and dibutyltin diacetate are added, and the material is discharged after stirring for 0.5h under vacuum.

[0024] Comparative Example 1 Comparative Example 1 provides a silane-modified polyether sealant, the main raw material composition of which is the same as that of Example 1, except that no modified filler and high-concentration silane masterbatch are added, but ordinary extender fillers and silane coupling agents are selected.

[0025] Comparative Example 2 Comparative Example 2 provides a silane-modified polyether sealant, the main raw material composition of which is the same as that of Example 1, except that no modified filler is added, but a common extender filler is selected.

[0026] Comparative Example 3 Comparative Example 3 provides a silane-modified polyether sealant, the main raw material composition of which is the same as that of Example 1, except that no high-concentration silane masterbatch is added, and a silane coupling agent is selected instead.

[0027] The performance tests were conducted on the silane-modified polyether sealants prepared in the above Examples 1 to 3 and Comparative Examples 1 to 3. The results are shown in Table 1.

[0028] Table 1 Performance test of silane modified polyether sealant Surface drying time (min) Curing depth (24h / mm) Initial adhesion (ball number) Consistency (cm) Tensile strength(MPa) Elongation at break (%) Example 1 23 3 18 8.3 3.5 510 Example 2 25 3 13 8.5 3.2 530 Example 3 20 3 16 8.2 3.3 475 Comparative Example 1 45 2 4 8.2 2.3 450 Comparative Example 2 33 2 8 8.4 2.1 440 Among them, the surface drying time is tested in accordance with GB / T13477; for the curing depth test, a 10mm thick strip is punched out, which is cut after 24 hours to measure its radius after curing; the initial adhesion test is to apply the silane-modified polyether sealant sample on a polyester film and quickly test it in accordance with GB / T 4852; the consistency test uses a putty consistency meter; the tensile strength and elongation at break are tested in accordance with GB / T528.

[0029] Table 2 Storage stability test Surface drying time (min) Curing depth (24h / mm) Consistency(cm) Example 1 33 2.5 8.0 Example 2 30 2.5 8.2 Example 3 31 2.5 8.1 Comparative Example 1 55 1.0 7.8 Comparative Example 2 40 1.0 7.5 The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0030] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A silane-modified polyether sealant for indoor doors and windows, characterized in that: The following raw materials are included in parts by weight: composition: Silane modified polyether polymer 26-40 parts Plasticizer 20-30 parts Modified filler 30-40 parts Antioxidant 0.1~1 part 1-2 parts of strengthening accelerator High concentration silane masterbatch 3-6 parts 1 to 3 parts of dewatering agent Catalyst 0.1-0.5 parts.

2. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The silane-modified polyether polymer is alkoxy-terminated polyether, dimethoxy-terminated polyether, diethoxy-terminated polyether and trimethoxy-terminated polyether.

3. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The plasticizer is a mixture of one or both of phthalates and polyether polyols; the modified filler is prepared by adding methylchlorosilane to the powder in steps, stirring and reacting at 150-180°C for 8-12 hours, then stirring for 3-5 hours under vacuum and constant temperature conditions, discharging the material after the reaction is completed, and grinding to obtain the modified filler, wherein the methylchlorosilane is dimethyldichlorosilane, and the powder is calcium carbonate.

4. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The antioxidant is a mixture of tris[2,4-di-tert-butylphenyl]phosphite, pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and n-octadecylβ-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

5. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The strengthening accelerator is rosin resin or terpene resin.

6. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The high-concentration silane masterbatch has a preparation method as follows: adding a silane coupling agent to paraffin in steps, stirring and reacting at 80-120°C for 1-2 hours, stirring for 15-30 minutes under vacuum and constant temperature conditions, cooling to room temperature and grinding after the reaction is completed to obtain a high-concentration silane masterbatch; the silane coupling agent is a mixture of one or more of γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, and N-aminoethyl-γ-aminopropyltriethoxysilane; the silane coupling agent is mixed and added in equal proportions, and the added amount of the silane coupling agent is 5-10%.

7. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The dewatering agent is a mixture of one or more of gamma-mercaptopropyltrimethoxysilane, vinyltrimethoxysilane and methyltrimethoxysilane.

8. The silane-modified polyether sealant for indoor doors and windows according to claim 1, characterized in that: The catalyst is a mixture of one or more of stannous octoate, dibutyltin dilaurate, dibutyltin diacetate and dibutyltin diacetylacetonate.

9. The silane-modified polyether sealant according to any one of claims 1 to 8, characterized in that: The preparation method thereof comprises the following steps: Weigh each raw material component according to the corresponding weight parts; The silane-modified polyether polymer, the plasticizer, the modified filler, the brightener, and the antioxidant are mixed uniformly; Add a strong accelerator, stir and dehydrate for 1 hour under the conditions of vacuum degree 0.09MPa~0.1MPa and temperature 100℃~120℃; Add high-concentration silane masterbatch and stir for 0.5h under the conditions of vacuum degree of 0.09MPa to 0.1MPa and temperature of 50℃ to 80℃; After cooling to below 50° C., a dehydrating agent and a catalyst are added, and the mixture is stirred under vacuum for 0.5 h to obtain the silane-modified polyether sealant.