High-flame-retardant fireproof sealant and preparation method thereof

Abstract

The invention belongs to the technical field of sealants, and relates to a high-flame-retardant fireproof sealant and a preparation method thereof.The sealant comprises, by weight, a component A: 10-20 parts of castor oil modified polyol I, 25-40 parts of castor oil modified polyol II, 5-15 parts of castor oil modified polyol III, 5-15 parts of polyether polyol I, 0.5-5 parts of an anti-settling agent and 0.5-5 parts of a dewatering agent; 0.3-1 part of a wetting dispersant, 20-50 parts of a flame-retardant and fireproof filler, 0.05-2 parts of a toner and 0.03-1 part of a catalyst; the component B is prepared from the following components in parts by weight: 10 to 30 parts of castor oil modified polyol I, 10 to 30 parts of polyether polyol II, 5 to 35 parts of isocyanate I and 5 to 30 parts of isocyanate II. The sealant disclosed by the invention is low in hardness, high in strength, low in viscosity, low in thermal conductivity, excellent in fireproof and flame-retardant performance, capable of effectively reducing generation of harmful gases and completely preventing invasion of flames, and safer and more reliable.

Description

Technical Field

[0001] The invention belongs to the technical field of sealants, and in particular relates to a highly flame-retardant and fireproof sealant and a preparation method thereof. Background Art

[0002] Fireproof sealants are widely used in the fields of construction, new energy, military industry, medical treatment, aviation, rail transportation, etc. With the development of these fields, the market demand for fireproof sealants will continue to grow. Especially in the field of construction, as a key material for achieving building fire safety, the market demand for fireproof sealants shows a steady growth trend.

[0003] The fireproof sealant industry is experiencing technological innovation, improving fireproof performance by introducing new flame retardants and optimizing polymer material modification technology. The innovation of fireproof sealants not only enhances the stability of materials at high temperatures, but also significantly improves their thermal insulation and flame retardancy, effectively extending the time that building components can maintain integrity during a fire. For example, some advanced fireproof sealant products still maintain excellent sealing effects under extreme conditions, buying precious escape time for people inside the building.

[0004] As global environmental awareness increases, the fireproof sealant industry has also responded positively and transformed towards green and environmental protection. The development of low-VOC (volatile organic compounds), non-toxic and harmless fireproof sealant products has become an industry consensus. These environmentally friendly products not only reduce the emission of harmful substances during the production process, but also reduce the potential harm to the environment and human body during use.

[0005] Fireproof sealants need further development and innovation, and their flame isolation capabilities need to be further improved. While being flame retardant in themselves, they should also be able to effectively reduce the generation of harmful gases and completely block the intrusion of flames. Summary of the invention

[0006] In view of the deficiencies of the above-mentioned prior art, the present invention provides a highly flame retardant fireproof sealant and a preparation method thereof. The specific technical scheme is as follows:

[0007] The first object of the present invention is to provide a highly flame retardant fireproof sealant, comprising component A and component B, calculated by weight:

[0008] Component A:

[0009] Castor oil modified polyol 1 10-20 parts, castor oil modified polyol 2 25-40 parts, castor oil modified polyol 3 5-15 parts, polyether polyol 1 5-15 parts, anti-settling agent 0.5-5 parts, dewatering agent 0.5-5 parts, wetting dispersant 0.3-1 parts, flame retardant and fireproof filler 20-50 parts, color powder 0.05-2 parts, catalyst 0.03-1 parts;

[0010] Component B:

[0011] Castor oil modified polyol 1 10-30 parts, polyether polyol 2 10-30 parts, isocyanate 1 5-35 parts, isocyanate 2 5-30 parts;

[0012] The castor oil modified polyol 1, castor oil modified polyol 2 and castor oil modified polyol 3 have different viscosities and hydroxyl values; the polyether polyol 1 and polyether polyol 2 have different molecular weights; the isocyanate 1 is liquefied MDI, and the isocyanate 2 is MDI-50;

[0013] The volume ratio of component A to component B is 1:1.

[0014] The present invention adopts different combinations of castor oil-modified polyols and polyether polyols from the perspective of molecular structure design, soft and hard segment combinations, and different molecular weights. The composed polymers form a complex and dense cross-linked network, thereby forming unique physical, chemical and mechanical properties of the glue.

[0015] Furthermore, the viscosity of the castor oil modified polyol 1 is 220mpa.s, and the hydroxyl value is 86mgKOH / g, such as HF-1300 of Ito Oil Mills, Ltd.; the viscosity of the castor oil modified polyol 2 is 3000mpa.s, and the hydroxyl value is 186mgKOH / g, such as Sovermol805 of BASF; the viscosity of the castor oil modified polyol 3 is 4000mpa.s, and the hydroxyl value is 180mgKOH / g, such as AC-006 of Ito Oil Mills, Ltd.

[0016] Furthermore, the polyether polyol 1 is one of a difunctional polyether polyol with a molecular weight of 400, a trifunctional polyether polyol with a molecular weight of 500 or a trifunctional polyether polyol with a molecular weight of 700, preferably a trifunctional polyether polyol with a molecular weight of 700, MN-700 of Shandong Bluestar Dongda Chemical Co., Ltd.; the polyether polyol 2 is a mixture of one or more difunctional polyether polyols with a molecular weight of 1000, 2000, 4000, 6000, 8000, 12000, preferably a difunctional polyether polyol with a molecular weight of 4000, such as DL-4000 of Shandong Bluestar Dongda Chemical Co., Ltd.

[0017] Furthermore, the anti-settling agent is one or more of a liquid anti-settling agent or fumed silica, preferably fumed silica, such as Wacker Chemical H2000; the dehydrating agent is one or more of a molecular sieve or an oxazolidine dehydrating agent, preferably 4A molecular sieve.

[0018] Furthermore, the wetting and dispersing agent is YRFC-06A produced by Guangzhou Yourun Chemical Co., Ltd.; and the color powder is carbon black.

[0019] Furthermore, the catalyst is one or more of an organic tin catalyst, an organic mercury catalyst, an organic zinc catalyst, an organic bismuth catalyst, and an organic nickel catalyst, preferably an organic zinc catalyst, such as CUCAT-EZ19 produced by Guangzhou Yourun Chemical Co., Ltd.

[0020] Furthermore, the flame retardant and fireproof filler is one or more of halogen-free phosphorus-based liquid flame retardant, phosphorus-based powder flame retardant, aluminum hydroxide, and expandable graphite.

[0021] Furthermore, the flame retardant and fireproof filler is a mixture of a halogen-free phosphorus-based liquid flame retardant, a phosphorus-based powder flame retardant and expandable graphite in a mass ratio of 3:6:7.

[0022] When the present invention adopts a mixture of halogen-free phosphorus liquid flame retardant, phosphorus powder flame retardant and expandable graphite in a mass ratio of 3:6:7 as a flame retardant and fireproof filler, the mixture has extremely low thermal conductivity, little viscosity increase on the system, excellent fireproof and flame retardant properties, and does not affect the mechanical properties and aging resistance of the glue, thereby achieving low thermal conductivity, low viscosity and super fireproof and flame retardant properties of the sealant.

[0023] Furthermore, the halogen-free phosphorus-based liquid flame retardant is Doher6000-5 from Doher Chemical Co., Ltd., the phosphorus-based powder flame retardant is ECP-6001 from Qingdao Ruinuo Technology Co., Ltd., and the expandable graphite is EG-150 from Qingdao Yanhai Carbon Materials Co., Ltd.

[0024] The second object of the present invention is to provide a method for preparing the above-mentioned highly flame retardant and fireproof sealant, comprising the following steps:

[0025] (1) Preparation of component A sealant: Castor oil modified polyol 1, castor oil modified polyol 2, castor oil modified polyol 3 1, and polyether polyol 1 are mixed evenly, and then an anti-settling agent, a water scavenger, a wetting dispersant, a flame retardant and fireproof filler and a color powder are added and mixed evenly, and finally a catalyst is added, and the mixture is degassed and stirred evenly to obtain the component A sealant;

[0026] (2) Preparation of component B sealant: castor oil modified polyol 1, polyether polyol 2, isocyanate 1 and isocyanate 2 are prepolymerized at 70-90° C. for 1-3 h to obtain the component B sealant.

[0027] When in use, component A and component B are mixed evenly in a volume ratio of 1:1, then poured onto the workpiece to be injected with glue, and then cured at room temperature or heated to 80°C or below.

[0028] The beneficial effects of the present invention are:

[0029] The present invention adopts castor oil-modified polyols and polyether polyols with different structures and molecular weights, as well as a flame-retardant and fire-proof filler mixed with a halogen-free phosphorus-based liquid flame retardant, a phosphorus-based powder flame retardant and expandable graphite, to obtain a sealant with low hardness, high strength, low viscosity, low thermal conductivity, excellent fire-retardant performance and no influence on the mechanical properties and aging resistance of the glue. The sealant can effectively reduce the generation of harmful gases and completely block the invasion of flames, and is safer and more reliable. DETAILED DESCRIPTION

[0030] The principles and features of the present invention are described below in conjunction with embodiments. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0031] Castor oil modified polyol 1: viscosity 220mPa.s, hydroxyl value 86mgKOH / g, HF-1300 from Ito Oil Manufacturing Co., Ltd.;

[0032] Castor oil modified polyol II: viscosity 3000mPa.s, hydroxyl value 186mgKOH / g, BASF's Sovermol805;

[0033] Castor oil modified polyol 3: viscosity 4000mPa.s, hydroxyl value 180mgKOH / g, AC-006 from Ito Oil Manufacturing Co., Ltd.;

[0034] Polyether polyol 1: trifunctional polyether MN-700 with a molecular weight of 700, Shandong Bluestar Dongda Chemical Co., Ltd.;

[0035] Polyether polyol 2: difunctional polyether polyol with a molecular weight of 4000, DL-4000 from Shandong Bluestar Dongda Co., Ltd.;

[0036] Anti-settling agent: fumed silica, Wacker Chemical H2000;

[0037] Dewatering agent: 4A molecular sieve;

[0038] Wetting and dispersing agent: Guangzhou Yourun Chemical Co., Ltd. YRFC-06A;

[0039] Toner: Carbon black;

[0040] Catalyst: Organic zinc catalyst, CUCAT-EZ19 from Guangzhou Yourun Chemical Co., Ltd.

[0041] Isocyanate 1 is liquefied MDI;

[0042] Isocyanate II is MDI-50;

[0043] Halogen-free phosphorus liquid flame retardant: Doher6000-5 from Doher Chemical Co., Ltd.

[0044] Phosphorus powder flame retardant: Qingdao Ruinuo Technology Co., Ltd. ECP-6001;

[0045] Expandable graphite: EG-150 from Qingdao Yanhai Carbon Materials Co., Ltd.;

[0046] The above material components are used in the following examples and comparative examples.

[0047] Example 1

[0048] Preparation of a highly flame retardant fireproof sealant:

[0049] Weigh 15.0 g of castor oil modified polyol 1, 34.0 g of castor oil modified polyol 2, 10.0 g of castor oil modified polyol 3, and 10.0 g of polyether polyol 1, mix them evenly, then add 2.5 g of anti-settling agent, 2.0 g of dewatering agent, 0.6 g of wetting dispersant, 6.0 g of halogen-free phosphorus liquid flame retardant, 12.0 g of phosphorus powder flame retardant, 14.0 g of expandable graphite, and 0.5 g of color powder, mix them evenly, and finally add 0.5 g of catalyst, degas, mix and stir evenly to obtain the A component sealant;

[0050] Weigh 25.0 g of castor oil-modified polyol 1, 25.0 g of polyether polyol 2, 35.0 g of isocyanate 1, and 15.0 g of isocyanate 2, and prepolymerize them at 80° C. for 2 h to obtain the B component sealant.

[0051] When in use, mix the two components evenly in a volume ratio of 1:1, then pour the glue on the workpiece to be injected and cure.

[0052] Example 2

[0053] Preparation of a highly flame retardant fireproof sealant:

[0054] Weigh 14.0 g of castor oil modified polyol 1, 35.0 g of castor oil modified polyol 2, 11.0 g of castor oil modified polyol 3, and 9.0 g of polyether polyol 1, mix them evenly, then add 2.5 g of anti-settling agent, 2.0 g of dewatering agent, 0.6 g of wetting dispersant, 6.0 g of halogen-free phosphorus liquid flame retardant, 12.0 g of phosphorus powder flame retardant, 14.0 g of expandable graphite, and 0.5 g of color powder, mix them evenly, and finally add 0.5 g of catalyst, degas, mix and stir evenly to obtain the A component sealant;

[0055] Weigh 25.0 g of castor oil-modified polyol 1, 25.0 g of polyether polyol 2, 35.0 g of isocyanate 1, and 15.0 g of isocyanate 2, and prepolymerize them at 80° C. for 2 h to obtain the B component sealant.

[0056] When in use, mix the two components in a volume ratio of 1:1 and pour the glue on the workpiece to be injected, and then allow to solidify.

[0057] Comparative Example 1

[0058] Preparation of a flame retardant fireproof sealant:

[0059] Weigh 15.0 g of castor oil modified polyol 1, 34.0 g of castor oil modified polyol 2, 10.0 g of castor oil modified polyol 3, and 10.0 g of polyether polyol 1, mix them evenly, then add 2.5 g of anti-settling agent, 2.0 g of dewatering agent, 0.6 g of wetting dispersant, 3.0 g of halogen-free phosphorus liquid flame retardant, 15.0 g of phosphorus powder flame retardant, 14.0 g of expandable graphite, and 0.5 g of color powder, mix them evenly, and finally add 0.5 g of catalyst, degas, mix and stir evenly to obtain the A component sealant;

[0060] Weigh 25.0 g of castor oil-modified polyol 1, 25.0 g of polyether polyol 2, 35.0 g of isocyanate 1, and 15.0 g of isocyanate 2, and prepolymerize them at 80° C. for 2 h to obtain the B component sealant.

[0061] When in use, mix the two components evenly in a volume ratio of 1:1, then pour the glue on the workpiece to be injected and cure.

[0062] Comparative Example 2

[0063] Preparation of a flame retardant fireproof sealant:

[0064] Weigh 15.0 g of castor oil modified polyol 1, 34.0 g of castor oil modified polyol 2, 10.0 g of castor oil modified polyol 3, and 10.0 g of polyether polyol 1, mix them evenly, then add 2.5 g of anti-settling agent, 2.0 g of dewatering agent, 0.6 g of wetting dispersant, 6.0 g of halogen-free phosphorus liquid flame retardant, 9.0 g of phosphorus powder flame retardant, 17.0 g of expandable graphite, and 0.5 g of color powder, mix them evenly, and finally add 0.5 g of catalyst, degas, mix and stir evenly to obtain the A component sealant;

[0065] Weigh 25.0 g of castor oil-modified polyol 1, 25.0 g of polyether polyol 2, 35.0 g of isocyanate 1, and 15.0 g of isocyanate 2, and prepolymerize them at 80° C. for 2 h to obtain the B component sealant.

[0066] When in use, mix the two components evenly in a volume ratio of 1:1, then pour the glue on the workpiece to be injected and cure.

[0067] The sealants obtained in Examples 1 and 2 and Comparative Examples 1 and 2 were tested. The heat curing conditions were 80° C. and 24 hours of heating curing. The test method was carried out in accordance with (GB / T2794-1995), (GB / T7124-2008), (GB / T528-2009), GB 23864-2023 and other methods. The specific test data are as follows.

[0068] Table 1. Test results of sealant performance of examples and comparative examples

[0069]

[0070] It can be seen from the data in Table 1 that the sealant of the present invention has the characteristics of low hardness, high strength, low viscosity, low thermal conductivity, excellent fire retardant performance, etc. Compared with the flame retardant ratio of the comparative example, it maintains better mechanical properties of the glue, and has excellent fire retardant performance while having significantly lower thermal conductivity, which is safer and more reliable.

[0071] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A highly flame retardant fireproof sealant, characterized in that: Including component A and component B, by weight: Component A: Castor oil modified polyol 1 10-20 parts, castor oil modified polyol 2 25-40 parts, castor oil modified polyol 3 5-15 parts, polyether polyol 1 5-15 parts, anti-settling agent 0.5-5 parts, dewatering agent 0.5-5 parts, wetting dispersant 0.3-1 parts, flame retardant and fireproof filler 20-50 parts, color powder 0.05-2 parts, catalyst 0.03-1 parts; Component B: Castor oil modified polyol 1 10-30 parts, polyether polyol 2 10-30 parts, isocyanate 1 5-35 parts, isocyanate 2 5-30 parts; The castor oil modified polyol 1, castor oil modified polyol 2 and castor oil modified polyol 3 have different viscosities and hydroxyl values; the polyether polyol 1 and polyether polyol 2 have different molecular weights; the isocyanate 1 is liquefied MDI, and the isocyanate 2 is MDI-50; The volume ratio of component A to component B is 1:

1.

2. The highly flame retardant fireproof sealant according to claim 1, characterized in that: The viscosity of the castor oil modified polyol 1 is 220 mpa.s, and the hydroxyl value is 86 mgKOH / g; the viscosity of the castor oil modified polyol 2 is 3000 mpa.s, and the hydroxyl value is 186 mgKOH / g; the viscosity of the castor oil modified polyol 3 is 4000 mpa.s, and the hydroxyl value is 180 mgKOH / g.

3. The highly flame retardant fireproof sealant according to claim 1, characterized in that: The polyether polyol 1 is one of a difunctional polyether polyol with a molecular weight of 400, a trifunctional polyether polyol with a molecular weight of 500 or a trifunctional polyether polyol with a molecular weight of 700; the polyether polyol 2 is a mixture of one or more difunctional polyether polyols with a molecular weight of 1000, 2000, 4000, 6000, 8000, 12000.

4. The highly flame retardant fireproof sealant according to claim 3, characterized in that: The polyether polyol 1 is a trifunctional polyether polyol with a molecular weight of 700; the polyether polyol 2 is a difunctional polyether polyol with a molecular weight of 4000.

5. The highly flame retardant fireproof sealant according to claim 1, characterized in that: The anti-settling agent is one or more of a liquid anti-settling aid or fumed silica; the dehydrating agent is one or more of a molecular sieve or an oxazolidine dehydrating agent; the catalyst is one or more of an organic tin catalyst, an organic mercury catalyst, an organic zinc catalyst, an organic bismuth catalyst, and an organic nickel catalyst.

6. The highly flame retardant fireproof sealant according to claim 5, characterized in that: The anti-settling agent is fumed silica, the dehydrating agent is 4A molecular sieve, and the catalyst is an organic zinc catalyst.

7. The highly flame retardant fireproof sealant according to claim 1, characterized in that: The wetting and dispersing agent is YRFC-06A from Guangzhou Yourun Chemical Co., Ltd.; and the toner is carbon black.

8. The highly flame retardant fireproof sealant according to claim 1, characterized in that: The flame retardant and fireproof filler is one or more of halogen-free phosphorus liquid flame retardant, phosphorus powder flame retardant, aluminum hydroxide, and expandable graphite.

9. The highly flame retardant fireproof sealant according to claim 8, characterized in that: The flame retardant and fireproof filler is a mixture of a halogen-free phosphorus-based liquid flame retardant, a phosphorus-based powder flame retardant and expandable graphite in a mass ratio of 3:6:

7.

10. A method for preparing a highly flame retardant fireproof sealant as claimed in any one of claims 1 to 9, characterized in that: The steps include: (1) Preparation of component A sealant: Castor oil modified polyol 1, castor oil modified polyol 2, castor oil modified polyol 3 1, and polyether polyol 1 are mixed evenly, and then an anti-settling agent, a water scavenger, a wetting dispersant, a flame retardant and fireproof filler and a color powder are added and mixed evenly, and finally a catalyst is added, and the mixture is degassed and stirred evenly to obtain the component A sealant; (2) Preparation of component B sealant: castor oil modified polyol 1, polyether polyol 2, isocyanate 1 and isocyanate 2 are prepolymerized at 70-90° C. for 1-3 h to obtain the component B sealant.

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