CN110628379A - Flame-retardant polysulfide sealant - Google Patents
Flame-retardant polysulfide sealant Download PDFInfo
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- CN110628379A CN110628379A CN201911049128.6A CN201911049128A CN110628379A CN 110628379 A CN110628379 A CN 110628379A CN 201911049128 A CN201911049128 A CN 201911049128A CN 110628379 A CN110628379 A CN 110628379A
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- flame
- retardant
- polysulfide sealant
- polysulfide
- sealant
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J181/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Adhesives based on polysulfones; Adhesives based on derivatives of such polymers
- C09J181/04—Polysulfides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention relates to a flame-retardant polysulfide sealant, which is characterized in that: the sealant consists of the following components in percentage by mass: 18-50% of silane modified polysulfide rubber, 1-5% of flame retardant, 1-15% of tackifier, 3-20% of plasticizer, 1-3% of accelerator, 3-20% of filler, 1-5% of antioxidant and 1-3% of ultraviolet-proof agent. The flame-retardant polysulfide sealant has the advantages of good flame-retardant property, large viscosity adjustable range, small specific gravity, no corrosion to base materials such as aluminum materials, glass and the like, and easy construction.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to a flame-retardant polysulfide sealant.
Background
The elastic polysulfide rubber compound formed by vulcanization is widely used as a sealant in the industries of traffic, construction, petrochemical industry and the like. The known polysulfide sealant is a two-component sealing material prepared by taking polysulfide rubber as a matrix, adding a proper amount of filler, auxiliary agent and curing agent, and mechanically mixing. In modern industrial production, particularly in the building industry and vehicle applications, sealants are required to have dual functions of sealing and bonding, and also to have good aging resistance, fatigue resistance, flexibility and the like. Silicone, polyurethane and polysulfide sealants are mostly used as known building, automobile and high-speed train sealants. The silicone sealant has general adhesive property and higher cost; the polyurethane sealant has poor solvent resistance and atmospheric aging resistance. The polysulfide sealant has the characteristics of reasonable cost, good bonding performance, good weather resistance, good solvent resistance and the like, and becomes an important sealant.
Research and practice shows that the polysulfide sealant has certain weather resistance. Xenon lamp accelerated aging of the polysulfide sealant for 28 days is carried out by the royal astragalus and the like, and the tensile strength of the polysulfide sealant is basically unchanged (manual accelerated aging research of the polysulfide sealant and the fluorine-silicon sealant, reported by Nanjing university of aviation). But under the condition of ultraviolet aging for 500h, the tensile strength and the elongation at break of the polysulfide sealant can be reduced to 60 percent of the original tensile strength and elongation at break of the polysulfide sealant. In the natural environment of practical application, humidity, oxygen, ozone, ultraviolet rays and the like can all affect various performances of the polysulfide sealant, but a plurality of factors cooperate with aging to obviously reduce the weather resistance of the polysulfide sealant.
In general, the aging of the polymer material in the external environment is mainly an autocatalytic process according to a radical reaction mechanism. The polysulfide sealant is a saturated heterochain polymer, is not easy to cause an aging reaction, and has relatively good weather resistance. However, the free radical reaction has an autocatalytic effect, and long-term aging causes considerable adverse effects on the polysulfide sealant. So far, no report is found for increasing the weather resistance of the polysulfide sealant by adopting functional additives such as an antioxidant, an ultraviolet-proof agent and the like. Secondly, the raw materials of the sealant are flammable, so that certain potential safety hazard is caused, and therefore, the production process in the aspect of flame retardant property of the sealant needs to be improved so as to obtain the polysulfide sealant with high flame retardant property and high weather resistance.
Disclosure of Invention
In order to solve the problems that in the prior art, multiple factors are cooperated with aging to obviously reduce the weather resistance of the polysulfide sealant and the raw materials of the sealant are inflammable to cause certain potential safety hazards, the production process in the aspect of flame retardant property of the sealant needs to be improved, the invention provides the flame-retardant polysulfide sealant.
The flame-retardant polysulfide sealant is characterized in that: the sealant consists of the following components in percentage by mass: 18-50% of silane modified polysulfide rubber, 1-5% of flame retardant, 1-15% of tackifier, 3-20% of plasticizer, 1-3% of accelerator, 3-20% of filler, 1-5% of antioxidant and 1-3% of ultraviolet-proof agent.
In a preferred embodiment of the invention, the flame-retardant polysulfide rubber is prepared by reacting polysulfide rubber, a silane coupling agent, hydroxyl silicone oil and hydrogenated castor oil, wherein the ratio of parts of the polysulfide rubber, the silane coupling agent, the hydroxyl silicone oil and the hydrogenated castor oil is 80: 5: 12: 15; the reaction was mixed at a temperature of 155 ℃ for 0.5 h.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a mixture of flame-retardant graphite modified by taking a silane coupling agent as a modifier and antimony trioxide as a flame retardant; the average particle size of the flame-retardant graphite in the flame retardant is 1500-3000 meshes, and the average particle size of the antimony trioxide is 0.3-1 micron.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant comprises any one or a mixture of any more of rosin resin, phenolic resin, epoxy resin, polyvinyl butyral and terpene resin.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant comprises a plasticizer which is any one or a mixture of any several of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl citrate chloroparaffin.
In a preferred embodiment of the invention, the flame retardant polysulfide sealant is a flame retardant polysulfide sealant, and the accelerator is either diphenylguanidine or triethanolamine or a mixture of the two.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a mixture of nano calcium carbonate, light calcium carbonate, titanium dioxide and carbon black.
In a preferred embodiment of the invention, the antioxidant is 2, 6-di-tert-butyl-p-cresol.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a benzotriazole compound.
The flame-retardant polysulfide sealant disclosed by the invention is added with an antioxidant and an anti-ultraviolet agent to improve the weather resistance of the polymer. The antioxidant blocks, inhibits or delays the oxidation or automatic oxidation process of the polymer, and can inhibit the free radical reaction of the polysulfide sealant; the ultraviolet inhibitor can shield or absorb high-energy ultraviolet rays and avoid the ultraviolet rays from initiating free radicals in the polysulfide sealant. In addition, the mechanical properties of the high weather resistance polysulfide sealant, such as tensile strength and elongation at break, are obviously improved by simultaneously adding the antioxidant and the ultraviolet-proof agent. The antioxidant and the anti-ultraviolet agent have synergistic action, and can jointly act to improve the tensile strength and the elongation at break of the high-weather-resistance polysulfide sealant, so that the high-weather-resistance polysulfide sealant has better mechanical properties.
In a preferred embodiment of the invention, the preparation method of the flame-retardant polysulfide sealant comprises the following steps of; drying the filler, the flame retardant, the antioxidant and the ultraviolet-proof agent at 80-90 ℃ for 2 hours; and putting the dried filler, the flame retardant, the silane modified polysulfide rubber, the tackifier, the plasticizer and the accelerator into a kneading machine for uniform mixing, grinding the mixed paste by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the single-component flame-retardant polysulfide sealant.
Compared with the prior art, the invention has the beneficial effects that: 1. the flame-retardant polysulfide sealant disclosed by the invention is added with an antioxidant and an anti-ultraviolet agent to improve the weather resistance of the polymer. The antioxidant blocks, inhibits or delays the oxidation or automatic oxidation process of the polymer, and can inhibit the free radical reaction of the polysulfide sealant; the ultraviolet inhibitor can shield or absorb high-energy ultraviolet rays and avoid the ultraviolet rays from initiating free radicals in the polysulfide sealant. In addition, the mechanical properties of the high weather resistance polysulfide sealant, such as tensile strength and elongation at break, are obviously improved by simultaneously adding the antioxidant and the ultraviolet-proof agent. The antioxidant and the anti-ultraviolet agent have synergistic action, and can jointly act to improve the tensile strength and the elongation at break of the high-weather-resistance polysulfide sealant, so that the high-weather-resistance polysulfide sealant has better mechanical properties. 2. The flame-retardant polysulfide sealant disclosed by the invention is added with a flame retardant, so that the flame-retardant property of the sealant is improved; 3. the polysulfide sealant has the advantages of good adhesiveness, good weather resistance and simple preparation process.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
as shown in figure 1, the flame-retardant polysulfide sealant is characterized in that: the sealant consists of the following components in percentage by mass: 18-50% of silane modified polysulfide rubber, 1-5% of flame retardant, 1-15% of tackifier, 3-20% of plasticizer, 1-3% of accelerator, 3-20% of filler, 1-5% of antioxidant and 1-3% of ultraviolet-proof agent.
In a preferred embodiment of the invention, the flame-retardant polysulfide rubber is prepared by reacting polysulfide rubber, a silane coupling agent, hydroxyl silicone oil and hydrogenated castor oil, wherein the ratio of parts of the polysulfide rubber, the silane coupling agent, the hydroxyl silicone oil and the hydrogenated castor oil is 80: 5: 12: 15; the reaction was mixed at a temperature of 155 ℃ for 0.5 h.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a mixture of flame-retardant graphite modified by taking a silane coupling agent as a modifier and antimony trioxide as a flame retardant; the average particle size of the flame-retardant graphite in the flame retardant is 1500-3000 meshes, and the average particle size of the antimony trioxide is 0.3-1 micron.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant comprises any one or a mixture of any more of rosin resin, phenolic resin, epoxy resin, polyvinyl butyral and terpene resin.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant comprises a plasticizer which is any one or a mixture of any several of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl citrate chloroparaffin.
In a preferred embodiment of the invention, the flame retardant polysulfide sealant is a flame retardant polysulfide sealant, and the accelerator is either diphenylguanidine or triethanolamine or a mixture of the two.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a mixture of nano calcium carbonate, light calcium carbonate, titanium dioxide and carbon black.
In a preferred embodiment of the invention, the antioxidant is 2, 6-di-tert-butyl-p-cresol.
In a preferred embodiment of the invention, the flame-retardant polysulfide sealant is a benzotriazole compound.
The flame-retardant polysulfide sealant disclosed by the invention is added with an antioxidant and an anti-ultraviolet agent to improve the weather resistance of the polymer. The antioxidant blocks, inhibits or delays the oxidation or automatic oxidation process of the polymer, and can inhibit the free radical reaction of the polysulfide sealant; the ultraviolet inhibitor can shield or absorb high-energy ultraviolet rays and avoid the ultraviolet rays from initiating free radicals in the polysulfide sealant. In addition, the mechanical properties of the high weather resistance polysulfide sealant, such as tensile strength and elongation at break, are obviously improved by simultaneously adding the antioxidant and the ultraviolet-proof agent. The antioxidant and the anti-ultraviolet agent have synergistic action, and can jointly act to improve the tensile strength and the elongation at break of the high-weather-resistance polysulfide sealant, so that the high-weather-resistance polysulfide sealant has better mechanical properties.
In a preferred embodiment of the invention, the preparation method of the flame-retardant polysulfide sealant comprises the following steps of; drying the filler, the flame retardant, the antioxidant and the ultraviolet-proof agent at 80-90 ℃ for 2 hours; and putting the dried filler, the flame retardant, the silane modified polysulfide rubber, the tackifier, the plasticizer and the accelerator into a kneading machine for uniform mixing, grinding the mixed paste by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the single-component flame-retardant polysulfide sealant.
Example 2:
in this embodiment of the invention, the sealant comprises a component A and a component B, wherein the weight ratio of the component A to the component B is A: b is 10: 3;
in a preferred embodiment of the present invention, the a-component glue comprises: 100 parts by weight of liquid silane modified polysulfide rubber, 30 parts by weight of dibutyl phthalate, 10 parts by weight of chlorinated paraffin, tributyl citrate, 20 parts by weight of nano calcium carbonate, 15 parts by weight of sulfur, 10 parts by weight of silane modified hyperbranched polyimide, 15 parts by weight of triethanolamine and 10 parts by weight of polyvinyl butyral;
in a preferred embodiment of the present invention, the B-component glue comprises: 100 parts by weight of manganese dioxide, 10 parts by weight of a vulcanization accelerator, 30 parts by weight of titanium dioxide, 25 parts by weight of dioctyl phthalate, 10 parts by weight of tributyl citrate chloroparaffin, 20 parts by weight of silane-modified hyperbranched polybenzimidazole and 15 parts by weight of 2, 2' -bis (4-carboxyphenoxy) benzidine.
In a preferred embodiment of the present invention, the silane-modified hyperbranched polyimide is prepared from raw materials including an epoxy silane coupling agent and an amino-terminated hyperbranched polyimide.
In a preferred embodiment of the present invention, the preparation steps of the amino terminated hyperbranched polyimide are: sequentially adding a solvent N, N-dimethylformamide and a triamine monomer 2,4, 6-tris [4- (2-aminophenoxy) phenyl ] pyridine into a reaction kettle, stirring, dropwise adding 3,3 ', 4, 4' -diphenyl ether tetracarboxylic dianhydride, stirring for reacting at 35 ℃ for 16 hours to obtain hyperbranched polyamic acid, and then adding acetic anhydride and pyridine for chemical imidization to prepare the amino-terminated hyperbranched polyimide.
In a preferred embodiment of the present invention, the silane-modified hyperbranched polybenzimidazole is prepared from raw materials comprising an epoxy silane coupling agent and an amino-terminated hyperbranched polybenzimidazole.
In a preferred embodiment of the present invention, the amino-terminated hyperbranched polybenzimidazole is prepared by dissolving 0.16 mole of 3,3 ', 4, 4' -tetraaminodiphenylsulfone in 1000 g of polyphosphoric acid containing 85 wt% phosphorus pentoxide, adding 0.1 mole of 1, 3, 5-m-trimellitic acid to the reaction solution, reacting at 200 ℃ for 20 hours, cooling to room temperature, precipitating into water, neutralizing with ammonia, filtering, and vacuum drying at 100 ℃ to obtain the amino-terminated hyperbranched polybenzimidazole.
In a preferred embodiment of the invention, the preparation method of the silane modified hyperbranched polybenzimidazole is that 100 parts by weight of completely dried amino-terminated hyperbranched polybenzimidazole and 80 parts by weight of epoxy silane coupling agent are added into a container to be mixed, the mixture is stirred for 50min under the protection of nitrogen, heated to 100 ℃ to react for 3h, cooled to room temperature, and the solution is poured into methanol to precipitate; repeatedly washing with methanol to remove solvent, filtering, and oven drying at 80 deg.C for 24 hr in a vacuum oven.
In a preferred embodiment of the present invention, any one of bicyclo [2.2.2] oct-7-ene-2, 3, 5, 6-tetracarboxylic dianhydride, 3, 4, 9, 10-perylenetetracarboxylic anhydride, and 4,4 ' - (hexafluoroisopropylidene) diphthalic anhydride may be used as the 3,3 ', 4,4 ' -diphenylether tetracarboxylic dianhydride.
In a preferred embodiment of the invention, the components of the A-component glue are mixed at 50 ℃, mechanically stirred and dispersed at the speed of 1000 revolutions per minute, and repeatedly ground for 60 minutes until a uniform paste is obtained, thus obtaining the A-component glue.
In a preferred embodiment of the invention, the components of the B-component glue are mixed at 50 ℃, mechanically stirred and dispersed at the speed of 1000 revolutions per minute, and repeatedly ground for 60 minutes until a uniform paste is obtained, thus obtaining the B-component glue.
In a preferred embodiment of the invention, the component A glue and the component B glue are mixed according to the weight ratio of 10: 2-6, mixing uniformly, and using.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The flame-retardant polysulfide sealant is characterized in that: the sealant consists of the following components in percentage by mass: 18-50% of silane modified polysulfide rubber, 1-5% of flame retardant, 1-15% of tackifier, 3-20% of plasticizer, 1-3% of accelerator, 3-20% of filler, 1-5% of antioxidant and 1-3% of ultraviolet-proof agent.
2. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the silane modified polysulfide rubber is prepared by reacting polysulfide rubber, a silane coupling agent, hydroxyl silicone oil and hydrogenated castor oil, wherein the part ratio of the polysulfide rubber to the silane coupling agent to the hydroxyl silicone oil to the hydrogenated castor oil is 80: 5: 12: 15; the reaction was mixed at a temperature of 155 ℃ for 0.5 h.
3. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the flame retardant is a mixture of flame-retardant graphite and antimony trioxide, which are modified by taking a silane coupling agent as a modifier; the average particle size of the flame-retardant graphite in the flame retardant is 1500-3000 meshes, and the average particle size of the antimony trioxide is 0.3-1 micron.
4. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the tackifier is any one or a mixture of any more of rosin resin, phenolic resin, epoxy resin, polyvinyl butyral and terpene resin.
5. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the plasticizer is any one or a mixture of any more of dibutyl phthalate, dioctyl phthalate, butyl benzyl phthalate and tributyl chloroparaffin citrate.
6. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the accelerator is any one or a mixture of two of diphenyl guanidine and triethanolamine.
7. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the filler is a mixture of nano calcium carbonate, light calcium carbonate, titanium dioxide and carbon black.
8. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the antioxidant is 2, 6-di-tert-butyl-p-cresol.
9. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the ultraviolet-proof agent is a benzotriazole compound.
10. The flame-retardant polysulfide sealant according to claim 1, characterized in that: the preparation method of the flame-retardant polysulfide sealant comprises the following steps; drying the filler, the flame retardant, the antioxidant and the ultraviolet-proof agent at 80-90 ℃ for 2 hours; and putting the dried filler, the flame retardant, the silane modified polysulfide rubber, the tackifier, the plasticizer and the accelerator into a kneading machine for uniform mixing, grinding the mixed paste by a colloid mill, and dehydrating in a vacuum state by a reaction kettle to obtain the single-component flame-retardant polysulfide sealant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911049128.6A CN110628379A (en) | 2019-10-31 | 2019-10-31 | Flame-retardant polysulfide sealant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911049128.6A CN110628379A (en) | 2019-10-31 | 2019-10-31 | Flame-retardant polysulfide sealant |
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| CN110628379A true CN110628379A (en) | 2019-12-31 |
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| CN201911049128.6A Pending CN110628379A (en) | 2019-10-31 | 2019-10-31 | Flame-retardant polysulfide sealant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277125A (en) * | 2011-08-31 | 2011-12-14 | 辽宁双强塑胶科技开发有限公司 | Flame-retardant polysulfide sealant and preparation method thereof |
| CN102838964A (en) * | 2012-08-29 | 2012-12-26 | 浙江大学 | High-weather-fastness polysulfide sealant |
| US10035926B2 (en) * | 2016-04-22 | 2018-07-31 | PRC—DeSoto International, Inc. | Ionic liquid catalysts in sulfur-containing polymer compositions |
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2019
- 2019-10-31 CN CN201911049128.6A patent/CN110628379A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277125A (en) * | 2011-08-31 | 2011-12-14 | 辽宁双强塑胶科技开发有限公司 | Flame-retardant polysulfide sealant and preparation method thereof |
| CN102838964A (en) * | 2012-08-29 | 2012-12-26 | 浙江大学 | High-weather-fastness polysulfide sealant |
| US10035926B2 (en) * | 2016-04-22 | 2018-07-31 | PRC—DeSoto International, Inc. | Ionic liquid catalysts in sulfur-containing polymer compositions |
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Application publication date: 20191231 |