CN112680163A - Single-component modified silicone flame-retardant sealant and preparation method thereof - Google Patents
Single-component modified silicone flame-retardant sealant and preparation method thereof Download PDFInfo
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
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Images
Abstract
The invention discloses a single-component modified silicone flame-retardant sealant and a preparation method thereof, belonging to the field of high polymer materials. The single-component modified silicone flame-retardant sealant takes the siloxane-terminated polyether resin as a colloid skeleton raw material, not only meets the definition of the national standard on modified silicone, but also can effectively solve the problems of poor adhesion of the traditional silicone adhesive product to porous materials, precipitation pollution of silicone oil and incapability of surface coating; the halogen-free environment-friendly flame retardant is used, so that toxic gases such as hydrogen halide and the like are not released at high temperature under the condition of ensuring the flame retardant effect; the flame-retardant sealant product obtained by matching with other components such as the UV aging resistant agent, the plasticizer and the like also has good mechanical property, weather resistance and durability. The invention also provides a preparation method of the single-component modified silicone flame-retardant sealant, which has simple operation steps and low requirements on instruments and process conditions and can realize industrial large-scale production.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a single-component modified silicone flame-retardant sealant and a preparation method thereof.
Background
With the continuous development of the construction industry, novel construction modes are continuously developed, and the requirement on the flame retardant property of the sealant for the building is higher and higher. The fire resistance limit of steel is very short, generally only 15 minutes, and under the high temperature, the mechanical property of steel can be rapidly reduced, so that the building collapses, and serious casualties are caused. Compared with a concrete structure, the steel structure has poor fire resistance and corrosion resistance. Therefore, in order to improve the fire-retardant performance of steel structures, the sealant used therein is also required to have fire-retardant properties.
The market circulation flame-retardant sealant is mostly the traditional silicone type flame-retardant sealant, is applied to buildings such as steel structures and the like, and has the problems in several aspects: (1) the silicone oil is separated out, and the vertical flow pollution is generated; (2) the elongation is low, and the steel structure is not suitable for a seam with large deformation; (3) the environment-friendly performance is poor, and the bromine-containing flame retardant is used, so that toxic gas is released by high-temperature combustion, and people can die by suffocation; (4) the surface can not be used for painting, coating and other decorative coatings.
Patent CN109666446A discloses a flame-retardant modified silicone sealant and a preparation method thereof, wherein the raw material used in the method is hydroxyl-terminated polydimethylsiloxane which is a raw material, and the molecular structure of the flame-retardant modified silicone sealant is as follows:
however, the modified silicone is defined in GB/T14683-2017 Silicone and modified Silicone building seals: single-component and multi-component sealants which are cured at room temperature and contain silane-terminated polyethers as the main component. The molecular structure is as follows:
according to the comparison, the modified silicone sealant disclosed in patent CN109666446A is not a product defined by GB/T14683-2017 standard.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide the one-component modified silicone flame retardant sealant which meets the standard definition of GB/T14683-2017, is environment-friendly and pollution-free, has good flame retardance, strong aging resistance, high elongation and excellent coating property.
In order to achieve the purpose, the invention adopts the technical scheme that:
a single-component modified silicone flame-retardant sealant comprises the following components in parts by weight: 80-140 parts of organic resin, 50-70 parts of plasticizer, 1.2-3 parts of UV aging resistant agent, 100-140 parts of filler, 180-280 parts of flame retardant and 5-9 parts of silane coupling agent; the organic resin comprises dimethoxysilane terminated polyether (MS) resin and trimethoxy silane terminated polyether (MS) resin; the flame retardant comprises an aluminum hydroxide flame retardant, a nitrogen-silicon flame retardant, a phosphorus flame retardant and a nitrogen-phosphorus flame retardant.
The dimethoxy silane terminated polyether resin is used as a framework component of the sealant product, so that the elongation of the colloid can be effectively adjusted; the trimethoxy silane terminated polyether resin is used as a framework component, and the curing speed and the physical and chemical properties of the product are adjusted by adjusting the proportion of the trimethoxy silane terminated polyether resin to the framework component. The two resin components do not contain methyl silicone oil, and the problem of silicone oil pollution is not caused.
The single-component modified silicone flame-retardant sealant provided by the invention takes the siloxane-terminated polyether resin as a colloid skeleton raw material, not only meets the standard definition of GB/T14683-2017, but also can effectively improve the elongation and the curing property of the product by the mutual matching of the two resins; the halogen-free environment-friendly flame retardant is used, so that toxic gases such as hydrogen halide and the like are not released at high temperature under the condition of ensuring the flame retardant effect, and the environment is protected; by matching with other components such as the UV aging resistant agent, the plasticizer and the like, the obtained sealant product also has good mechanical property and coating property.
Preferably, the organic resin comprises the following components in parts by weight: 0-100 parts of dimethoxysilane terminated polyether resin and 20-100 parts of trimethoxy silane terminated polyether resin. The organic resin obtained by matching the proportion can further improve the elongation and the curing property of the single-component modified silicone flame-retardant sealant.
More preferably, the organic resin comprises the following components in parts by weight: 70-100 parts of dimethoxy silane terminated polyether resin and 25-50 parts of trimethoxy silane terminated polyether resin.
Preferably, the plasticizer is a plasticizer DINP. The addition of the DINP (diisononyl phthalate) can improve the processability of the sealant product.
Preferably, the UV aging resistant agent comprises the following components in parts by weight: 0.2-1 part of light stabilizer and 1-2 parts of ultraviolet absorber. The addition of the two components can improve the ultraviolet resistance of the prepared modified silicone sealant product after coating, thereby prolonging the service life of the product.
Preferably, the flame retardant comprises the following components in parts by weight: 50 to 80 parts of aluminum hydroxide flame retardant, 50 to 100 parts of nitrogen-silicon flame retardant, 40 to 60 parts of phosphorus flame retardant and 50 to 100 parts of nitrogen-phosphorus flame retardant. The flame retardant prepared by the proportion not only maintains excellent flame retardant property, but also is non-toxic, non-irritant and environment-friendly without adding harmful solvents such as halogen, aldehyde, benzene and the like.
Preferably, the filler is light calcium carbonate. The light calcium carbonate has much larger sedimentation volume than common calcium carbonate filler, and can effectively improve the overall physical properties of the material such as wear resistance, sagging property and the like when being used as colloid filler.
Preferably, the silane coupling agent comprises the following components in parts by weight: 3-5 parts of vinyl silane coupling agent, 1-2 parts of amino silane coupling agent and 1-2 parts of epoxy silane coupling agent. The vinyl silane coupling agent is mainly used for removing redundant moisture in the sealant product, so that the storage property and stability of the product are effectively improved; the compounding of the aminosilane coupling agent and the epoxy silane coupling agent can effectively improve the adhesion of the sealant product and make the product easier to use.
Preferably, the single-component modified silicone flame-retardant sealant further comprises the following components in parts by weight: 1-3 parts of thixotropic agent, 10-15 parts of color paste, 1-2 parts of antioxidant and 0.5-1.5 parts of catalyst. The mechanical property and the tolerance of the sealant product can be further improved and the product has beautiful color by adding the components.
Preferably, the thixotropic agent is fumed silica; the antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010); the catalyst is chelated tin. The fumed silica can effectively improve the sagging performance of the sealant product; the antioxidant 1010 is used as a common rubber product preparation additive, so that the heat resistance of the product in the using process can be improved; the chelated tin acts primarily as a hardener in the overall formulation, allowing the product to be shaped and remain stable.
The invention also aims to provide a preparation method of the single-component modified silicone flame-retardant sealant, which comprises the following steps:
(1) mixing and stirring organic resin, a UV aging resistant agent, a thixotropic agent, an antioxidant, color paste and part of plasticizer uniformly to obtain a precursor A; in the step, the addition amount of the organic resin accounts for half of the total weight of the organic resin in the components of the single-component modified silicone flame-retardant sealant;
(2) adding a filler and a flame retardant into the precursor A obtained in the step (1), uniformly stirring and mixing, heating and decompressing, continuously stirring for 90-120 min, and cooling to obtain a precursor B;
(3) adding the residual addition amount of organic resin and plasticizer into the precursor B obtained in the step (2), stirring for 4-6 min, reducing pressure, and continuously stirring for 10-15 min to obtain a precursor C;
(4) and (4) adding a silane coupling agent and an activator into the precursor C obtained in the step (3), stirring for 3-5 min, reducing the pressure, and continuously stirring for 25-35 min to obtain the single-component modified silicone flame-retardant sealant.
The preparation method of the single-component modified silicone flame-retardant sealant provided by the invention has the advantages of simple operation steps, low requirements on instruments and process conditions, and realization of industrial large-scale production.
Preferably, the heating temperature in the step (2) is more than or equal to 80 ℃. The temperature can remove moisture contained in each component, and the long-term storage of the product is facilitated.
Preferably, the pressure after the pressure reduction in the steps (2) to (4) is less than or equal to-0.08 MPa. Under the condition, all the components are stirred and mixed more fully.
The invention has the beneficial effects that: the invention provides a single-component modified silicone flame-retardant sealant, which takes siloxane-terminated polyether resin as a colloid framework raw material, not only meets the definition of national standard on modified silicone, but also can effectively improve the elongation and the curing property of the product by the mutual matching of the two resins; the halogen-free environment-friendly flame retardant is used, so that toxic gases such as hydrogen halide and the like are not released at high temperature under the condition of ensuring the flame retardant effect, and the environment is protected; by matching with other components such as the UV aging resistant agent, the plasticizer and the like, the obtained sealant product also has good mechanical property and coating property. The invention also provides a preparation method of the single-component modified silicone flame-retardant sealant, which has simple operation steps and low requirements on instruments and process conditions and can realize industrial large-scale production.
Drawings
FIG. 1 is a comparison schematic diagram of the water pollution test results of the single-component modified silicone flame-retardant sealant prepared by the invention and the comparison traditional silicone flame-retardant sealant.
FIG. 2 is a schematic comparison of the results of the surface coating wettability tests of the single-component modified silicone flame retardant sealant prepared by the present invention and a comparative conventional silicone flame retardant sealant.
Detailed Description
For better illustrating the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples, which are intended to be understood in detail, but not intended to limit the present invention.
Unless otherwise specified, the raw materials used in the following examples are all commercially available common products.
Examples 1 to 10
The component formulas of the single-component modified silicone flame-retardant sealant disclosed by the invention are shown in the table 1. The preparation method of the product of each embodiment is the same, and comprises the following steps:
(1) adding organic resin, an UV aging resistant agent, a thixotropic agent, an antioxidant, a plasticizer and color paste into a planetary mixer, mixing and stirring at a speed of 10r/min for 5min to be uniform, and obtaining a precursor A; in the step, the addition amount of the organic resin and the plasticizer accounts for half of the total content of the organic resin and the plasticizer in the single-component modified silicone flame-retardant sealant component;
(2) adding the filler and the flame retardant into the precursor A obtained in the step (1) at 25r/min, stirring and mixing for 30min to be uniform, heating to 85 ℃, reducing the pressure to-0.08 MPa, continuing stirring for 120min, and cooling to 50 ℃ to obtain a precursor B;
(3) adding the residual addition amount of organic resin and plasticizer into the precursor B obtained in the step (2), stirring for 5min at a speed of 20r/min, reducing the pressure to-0.08 MPa, and continuously stirring for 10min to obtain a precursor C;
(4) and (4) adding a silane coupling agent and an activator into the precursor C obtained in the step (3), stirring for 5min at a speed of 15r/min, reducing the pressure to-0.08 MPa, and continuously stirring for 30min to obtain the single-component modified silicone flame-retardant sealant.
TABLE 1
TABLE 2
Comparative examples 1 to 8
The modified sealant in the comparative example is different from the modified sealants in examples 1 to 10 only in the content of each component, and the formula of the sealant is shown in Table 3.
TABLE 3
Effect example 1
In order to verify the mechanical properties and flame retardancy of the single-component modified silicone flame-retardant sealant, the products obtained in examples 1-4 and comparative examples 1-8 were tested, and meanwhile, the commercially available domestic silicone adhesive flame-retardant sealant was used as a control group, and the test methods, test items and test results are shown in table 4.
TABLE 4
As can be seen from Table 4, compared with the modified sealant obtained in the comparative example and the existing commercially available flame retardant adhesive, the single-component modified silicone flame retardant sealant obtained in the embodiment of the invention has better stretchability, and ensures that the sealant has good deformation following performance; the thermal expansion coefficient of the general steel material is 10 x 10-6The size of the joint varies with temperature, and a typical flame retardant glue is not suitable for such steel structures due to its low elongation compared to the products according to the invention. In addition, the product of the invention also has good heat resistance and flame retardance.
In order to verify the environmental protection property, the stability and the coating property of the single-component modified silicone flame-retardant sealant, the product obtained in the example 1 and the commercially available silicone adhesive flame-retardant sealant are subjected to a V-shaped water-splashing pollution experiment and a sealant surface coating wettability test together, wherein the test method of the test is a SUNSTAR enterprise standard test method.
The test results are respectively shown in fig. 1 and fig. 2, and the single-component modified silicone flame-retardant sealant does not contain silicone oil and contains a modified additive for improving stability, so that the single-component modified silicone flame-retardant sealant does not have a precipitation pollution phenomenon after being exposed outdoors for 30 days compared with the traditional commercially available flame-retardant sealant; when the paint wettability test is carried out, compared with the traditional silicone adhesive flame-retardant adhesive, the surface energy of the paint is higher, and the viscosity of the paint is not influenced when the paint is wetted on the surface of the paint.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The single-component modified silicone flame-retardant sealant is characterized by comprising the following components in parts by weight: 80-140 parts of organic resin, 50-70 parts of plasticizer, 1.2-3 parts of UV aging resistant agent, 100-150 parts of filler, 180-280 parts of flame retardant and 5-9 parts of silane coupling agent; the organic resin comprises dimethoxysilane terminated polyether resin and trimethoxy silane terminated polyether resin; the flame retardant comprises an aluminum hydroxide flame retardant, a nitrogen-silicon flame retardant, a phosphorus flame retardant and a nitrogen-phosphorus flame retardant.
2. The one-component modified silicone flame retardant sealant of claim 1, wherein the organic resin comprises the following components in parts by weight: 0-100 parts of dimethoxysilane terminated polyether resin and 25-100 parts of trimethoxy silane terminated polyether resin; preferably, the organic resin comprises the following components in parts by weight: 70-100 parts of dimethoxy silane terminated polyether resin and 25-50 parts of trimethoxy silane terminated polyether resin.
3. The one-component modified silicone flame retardant sealant of claim 1 wherein the plasticizer is the plasticizer DINP.
4. The one-component modified silicone flame retardant sealant of claim 1, wherein the UV aging resistant agent comprises the following components in parts by weight: 0.2-1 part of light stabilizer and 1-2 parts of ultraviolet absorber.
5. The one-component modified silicone flame retardant sealant according to claim 1, wherein the flame retardant comprises the following components in parts by weight: 50 to 80 parts of aluminum hydroxide flame retardant, 50 to 100 parts of nitrogen-silicon flame retardant, 40 to 60 parts of phosphorus flame retardant and 50 to 100 parts of nitrogen-phosphorus flame retardant.
6. The one-part modified silicone flame retardant sealant of claim 1 wherein the filler is precipitated calcium carbonate.
7. The one-component modified silicone flame retardant sealant of claim 1, wherein the silane coupling agent comprises the following components in parts by weight: 3-5 parts of vinyl silane coupling agent, 1-2 parts of amino silane coupling agent and 1-2 parts of epoxy silane coupling agent.
8. The single component modified silicone flame retardant sealant of claim 1, further comprising the following components in parts by weight: 1-3 parts of thixotropic agent, 10-15 parts of color paste, 1-2 parts of antioxidant and 0.5-1.5 parts of catalyst.
9. The one-part modified silicone flame retardant sealant of claim 8 wherein the thixotropic agent is fumed silica; the antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the catalyst is chelated tin.
10. The preparation method of the single-component modified silicone flame retardant sealant as claimed in any one of claims 1 to 9, characterized by comprising the following steps:
(1) mixing and stirring organic resin, a UV aging resistant agent, a thixotropic agent, an antioxidant, color paste and part of plasticizer uniformly to obtain a precursor A; in the step, the addition amount of the organic resin accounts for half of the total weight of the organic resin in the components of the single-component modified silicone flame-retardant sealant;
(2) adding a filler and a flame retardant into the precursor A obtained in the step (1), uniformly stirring and mixing, heating and decompressing, continuously stirring for 90-120 min, and cooling to obtain a precursor B;
(3) adding the residual addition amount of organic resin and plasticizer into the precursor B obtained in the step (2), stirring for 4-6 min, reducing pressure, and continuously stirring for 10-15 min to obtain a precursor C;
(4) and (4) adding a silane coupling agent and an activator into the precursor C obtained in the step (3), stirring for 3-5 min, reducing the pressure, and continuously stirring for 25-35 min to obtain the single-component modified silicone flame-retardant sealant.
Priority Applications (1)
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113817439A (en) * | 2021-09-29 | 2021-12-21 | 山东福瑞斯新材料科技有限公司 | Flame-retardant modified silicone building sealant and preparation method thereof |
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CN105368366A (en) * | 2015-12-15 | 2016-03-02 | 山东北方现代化学工业有限公司 | Silane-terminated polyether sealant and preparation method thereof |
CN109679572A (en) * | 2018-12-29 | 2019-04-26 | 广州市白云化工实业有限公司 | The silicone fireproof seal gum and preparation method thereof of the low high displacement capacity of modulus |
CN111117518A (en) * | 2019-12-13 | 2020-05-08 | 北京东方雨虹防水技术股份有限公司 | Mildew-proof bactericide, long-acting mildew-proof modified silicone mildew-proof sealant in service period and preparation method thereof |
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CN105368366A (en) * | 2015-12-15 | 2016-03-02 | 山东北方现代化学工业有限公司 | Silane-terminated polyether sealant and preparation method thereof |
CN109679572A (en) * | 2018-12-29 | 2019-04-26 | 广州市白云化工实业有限公司 | The silicone fireproof seal gum and preparation method thereof of the low high displacement capacity of modulus |
CN111117518A (en) * | 2019-12-13 | 2020-05-08 | 北京东方雨虹防水技术股份有限公司 | Mildew-proof bactericide, long-acting mildew-proof modified silicone mildew-proof sealant in service period and preparation method thereof |
Cited By (1)
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CN113817439A (en) * | 2021-09-29 | 2021-12-21 | 山东福瑞斯新材料科技有限公司 | Flame-retardant modified silicone building sealant and preparation method thereof |
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