Tough organic silicon fireproof microcapsule fire extinguishing tablet and preparation method thereof

Abstract

The invention belongs to the technical field of fire extinguishing tablets, and particularly relates to a tough organic silicon fireproof microcapsule fire extinguishing tablet and a preparation method thereof. The tough type organic silicon fireproof microcapsule fire extinguishing sheet provided by the invention is prepared from the following raw materials in parts by mass: 50 to 80 parts of double-end vinyl silicone oil, 10 to 40 parts of end-side vinyl silicone oil, 30 to 80 parts of reinforced resin, 1 to 10 parts of hydrogen-containing silicone oil, 0.2 to 0.6 part of platinum catalyst, 0.01 to 0.04 part of inhibitor, 0.5 to 5 parts of reinforcing filler, 1 to 5 parts of pigment and 200 to 300 parts of fireproof microcapsule. The organic silica gel is used as a base material of the fire extinguishing sheet, a high curing temperature is not needed, curing can be completed after heat preservation is conducted for 30 min at 60 DEG C, release of a fire extinguishing agent in the microcapsule cannot be caused, and therefore the fire extinguishing effect of the product is greatly improved.

Description

Technical Field

[0001] The present application belongs to the technical field of fire extinguishing tablets, and in particular relates to a tough organic silicon fireproof microcapsule fire extinguishing tablet and a preparation method thereof. Background Art

[0002] Fire extinguishers are common firefighting equipment used to extinguish early-stage fires. When used correctly, they can quickly contain a fire and prevent it from becoming a major disaster. Existing fire extinguishers are bulky, inconvenient to use, and difficult to carry around. To adapt to diverse firefighting scenarios, researchers have developed innovative firefighting devices—fire extinguishing tablets—that can be attached to indoor walls or ceilings. When a fire breaks out, the extinguishing agent within the tablet is released to extinguish the flames. Perfluorohexanone microcapsules are commonly used as the extinguishing agent, as they have a low heat of evaporation, easily vaporize, and rapidly absorb heat, effectively extinguishing the fire.

[0003] Existing fire-extinguishing tablets typically mix perfluorohexanone microcapsules with a base material, then heat and cure to form the finished product. This base material is often made of a thermosetting adhesive, such as polyurethane. For example, patent CN116920318B discloses a fire-extinguishing microcapsule and its production method. The surface of the fire-extinguishing microcapsule particles is coated with a film of silicone, polyurethane, epoxy resin, or other materials. When heated to high temperatures, high pressure builds up inside the microcapsule, causing the film to partially rupture, allowing the fire extinguishing agent to be ejected at high pressure from the damaged, weak areas. Polyurethane glue cures slowly and requires higher temperatures to cure quickly. The fire extinguishing agent inside the microcapsules is easily released at high temperatures, thereby reducing the fire extinguishing effect. In addition, thermosetting glue has poor aging resistance and corrosion resistance and cannot be used for a long time. It is usually necessary to spray a layer of polymer on the surface of the fire extinguishing piece to form a protective film, but the polymer on the surface will inhibit the release of the fire extinguishing agent inside the microcapsules, thereby reducing the fire extinguishing efficiency of the fire extinguishing piece. Moreover, although the fire extinguishing piece using thermosetting glue as the matrix has a certain strength, it is very brittle and has very poor toughness, and is prone to breakage when bent or stretched.

[0004] Based on the above analysis, it is very important to provide a fire-resistant microcapsule fire extinguishing sheet with high strength and toughness that will not be easily broken or damaged during use. Summary of the Invention

[0005] The embodiment of the present application provides a tough organic silicone fireproof microcapsule fire extinguishing sheet to solve the problems in the related art that the existing base material has a slow curing speed, cures quickly at high temperature but the microcapsules are easily released, and the base material has poor aging resistance and corrosion resistance, and the fire extinguishing sheet is brittle and has poor toughness.

[0006] In the first aspect, the present application provides a tough organic silicone fireproof microcapsule fire extinguishing sheet, which includes the following raw materials in parts by mass: 50 to 80 parts of double-ended vinyl silicone oil, 10 to 40 parts of end-side vinyl silicone oil, 30 to 80 parts of reinforcing resin, 1 to 10 parts of hydrogen-containing silicone oil, 0.2 to 0.6 parts of platinum catalyst, 0.01 to 0.04 parts of inhibitor, 0.5 to 5 parts of reinforcing filler, 1 to 5 parts of pigment, and 200 to 300 parts of fireproof microcapsules.

[0007] In some embodiments, the fireproof microcapsules include a core material and a shell material coated on the core material; wherein the core material is a perfluorinated fire extinguishing agent, and the shell material is a non-porous polymer containing an active modifier.

[0008] In some embodiments, the perfluorinated fire extinguishing agent is a mixture of one or more of perfluorohexanone, perfluorotriethylamine, tetrafluorodibromoethane, difluorobromochloromethane, difluorodichloroethane, difluorotrichloroethane, 2-iodo-heptafluoropropane, 1-iodo-heptafluoropropane, and trifluorotrichloroethane. The active modifier is at least one of a vinyl monomer or polymer, acrylic acid, methacrylic acid, acrylate, acrylic acid-modified polyurethane, and acrylic acid-modified silicone resin.

[0009] In some preferred embodiments, the perfluorinated fire extinguishing agent is perfluorohexanone.

[0010] In some embodiments, the vinyl groups of the double-ended vinyl silicone oil are at both ends of the silicone oil long chain, and the viscosity at 25°C is 500-10000 mPa·s; the vinyl groups of the side-terminated vinyl silicone oil are at both ends and on the side chain of the silicone oil long chain, and the viscosity at 25°C is 100-2000 mPa·s; the viscosity of the hydrogen-containing silicone oil is 100-2000 mPa·s, and the hydrogen content is 0.6%-1.6%.

[0011] In some embodiments, the reinforcing resin is an MQ resin containing vinyl groups, and the M / Q ratio is 0.8 to 1.2.

[0012] In some embodiments, the platinum catalyst is a mixture of any one or more of chloroplatinic acid-divinyltetramethyldisiloxane, chloroplatinic acid-isopropyl alcohol, and chloroplatinic acid-diethyl phthalate.

[0013] In some embodiments, the inhibitor is a mixture of any one or more of methyl acetylene alcohol, methyl butynol, methyl pentynol, and ethynyl cyclohexanol.

[0014] In some embodiments, the reinforcing filler is hydrophobic silica; and the pigment is oily orange paste and yellow paste.

[0015] In a second aspect, the present application also provides a method for preparing the above-mentioned tough organic silicon fireproof microcapsule fire extinguishing tablet, comprising the following steps:

[0016] Step S101: Add bi-terminal vinyl silicone oil, end-side vinyl silicone oil, reinforcing resin, and inhibitor into a reaction kettle, and stir at room temperature for 5 to 10 minutes at a speed of 50 r / min to obtain a first mixture;

[0017] Step S102: adding hydrogen-containing silicone oil, reinforcing filler, and pigment to the first mixture, stirring at room temperature for 5 to 10 minutes at a speed of 50 rpm to obtain a second mixture;

[0018] Step S103: Continue stirring, add the platinum catalyst to the second mixture while stirring, and stir at room temperature for 5 to 10 minutes at a speed of 50 r / min until the mixture is evenly dispersed to obtain a third mixture;

[0019] Step S104: adding the fireproof microcapsules to the third mixture, stirring at room temperature for 5 to 10 minutes at a speed of 50 rpm to uniformly disperse the mixture; vacuum degassing the uniformly dispersed rubber for 1 hour, stopping stirring, and discharging the rubber;

[0020] Step S105: Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60°C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60°C drying tunnel, cure for 30 minutes, remove from the drying tunnel, and demold to obtain the tough organic silicone fire-retardant microcapsule fire extinguishing sheet.

[0021] In some embodiments, the fire-resistant microcapsules are prepared by the following process: adding a perfluorinated fire extinguishing agent to an emulsifier solution, then adding a shell material prepolymer, adding citric acid to adjust the pH value, and then adding an active modifier to react to obtain a microcapsule emulsion; the microcapsule emulsion is sieved and dried to obtain the fire-resistant microcapsules.

[0022] In some embodiments, the fire-resistant microcapsules are prepared by the following process:

[0023] S201, mixing melamine and formaldehyde aqueous solution, adding triethanolamine to adjust the pH value, heating in a water bath, and stirring to obtain a shell material prepolymer;

[0024] S202, adding citric acid to the styrene-maleic anhydride solution to adjust the pH, then adding sodium perfluorononyloxybenzenesulfonate, stirring and dispersing uniformly to obtain an emulsifier solution;

[0025] S203, adding a perfluorinated fire extinguishing agent to the emulsifier solution, dispersing the mixture, and obtaining a mixed emulsion;

[0026] S204, adding the shell material prepolymer to the mixed emulsion, adding citric acid to adjust the pH value, and then adding an active modifier to react to obtain a microcapsule emulsion;

[0027] S205, sieving the microcapsule emulsion and drying it to obtain fireproof microcapsules.

[0028] In some embodiments, in step S201, triethanolamine is added to adjust the pH value to 8-9, and the temperature of the water bath heating is 70-90° C.; in step S202, citric acid is added to adjust the pH value to 4-5.

[0029] In some embodiments, in step S204, citric acid is added to adjust the pH value to 4-5; in step S205, the drying temperature is 40-50°C.

[0030] The fire extinguishing sheet prepared in the present application can be attached to a wall or ceiling and can be widely used in indoor places where fire may occur. The fire extinguishing sheet has excellent fireproof performance and high strength and toughness, and will not be easily broken or damaged during use.

[0031] The beneficial effects of the technical solution provided by this application include:

[0032] 1. This application uses organic silica gel as the base material of the fire extinguishing sheet, which does not require a high curing temperature. Curing can be completed by keeping it at 60°C for 30 minutes. It will not cause the release of the fire extinguishing agent inside the microcapsule, thereby greatly improving the fire extinguishing effect of the product;

[0033] 2. Silicone has good aging resistance and corrosion resistance. There is no need to spray a layer of polymer protective film on the surface of the fire extinguishing piece. The fire extinguishing agent inside the microcapsule can be released better, thereby greatly improving the fire extinguishing efficiency of the product.

[0034] 3. This application reduces the crosslinking density of the system and adds a small amount of hydrophobic silica to improve toughness. By adding reinforcing resin to improve strength, a fire extinguishing tablet product with both strength and toughness is obtained. The fire extinguishing tablet product of this application has a tensile strength of up to 0.96 MPa and an elongation at break of up to 97%;

[0035] 4. The surface of the fireproof microcapsules used in this application contains a large number of active vinyl groups. When added to organic silica gel water, under the action of platinum catalyst, the active vinyl groups on the surface of the microcapsules will undergo a silylation reaction with hydrogen-containing silicone oil, so that the microcapsules and organic silica gel water have good compatibility, avoiding problems such as phase separation; the microcapsules and glue have good chemical bonding, which can effectively improve the fire extinguishing performance and mechanical properties of the fire extinguishing sheet, while ensuring that the fire extinguishing sheet maintains its integrity after the microcapsules are released to avoid residue splashing. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0037] Figure 1 Schematic diagram of the principle of combining fire-retardant microcapsules and silicone oil used in this application. DETAILED DESCRIPTION

[0038] To make the purpose, technical solutions, and advantages of the embodiments of this application more clear, the technical solutions in the embodiments of this application will be clearly and completely described below in conjunction with the drawings in the embodiments of this application. Obviously, the described embodiments are part of the embodiments of this application, not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0039] The embodiment of the present application provides a tough organic silicone fireproof microcapsule fire extinguishing sheet, which can solve the problems of the existing base material having a slow curing speed, fast curing at high temperature but easy release of microcapsules, poor aging resistance and corrosion resistance of the base material, and the brittleness and poor toughness of the fire extinguishing sheet.

[0040] The present invention provides a method for preparing a tough organic silicon fireproof microcapsule fire extinguishing tablet, comprising the following steps, wherein the following amounts are calculated in parts by mass:

[0041] Step S101, adding 50-80 parts of bi-end vinyl silicone oil, 10-40 parts of end vinyl silicone oil, 30-80 parts of reinforcing resin, and 0.01-0.04 parts of inhibitor into a reactor, stirring for 5-10 minutes at room temperature and a speed of 50 r / min to obtain a uniform dispersion, thereby obtaining a first mixture;

[0042] Step S102: adding 1 to 10 parts of hydrogenated silicone oil, 0.5 to 5 parts of reinforcing filler, and 1 to 5 parts of pigment to the first mixture, stirring for 5 to 10 minutes at room temperature and a rotation speed of 50 rpm to obtain a second mixture;

[0043] Step S103, continue stirring, add 0.2 to 0.6 parts of platinum catalyst to the second mixture while stirring, stir at room temperature for 5 to 10 minutes, rotate at 50 rpm, and disperse evenly to obtain a third mixture;

[0044] Step S104: adding 200 to 300 parts of the fireproof microcapsules to the third mixture, stirring at room temperature for 5 to 10 minutes at a speed of 50 r / min to disperse evenly; vacuum degassing the evenly dispersed rubber material for 1 hour, stopping stirring, and discharging the rubber material;

[0045] Step S105: Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60°C, adjust the distance between the upper and lower rollers of the calender to 2mm, start the calender, move the rubber material to the 60°C drying tunnel, cure for 30 minutes, remove from the drying tunnel, demold, and obtain the fire extinguishing sheet product.

[0046] Among them, fireproof microcapsules are prepared by the following process:

[0047] 30g of melamine and 60g of a 37% formaldehyde aqueous solution were added to a three-necked flask, triethanolamine was added dropwise to adjust the pH to 8-9, and the mixture was heated in a water bath to 70-90°C. The mixture was stirred for 1.5h and then discharged to obtain a colorless, clear and transparent melamine resin prepolymer.

[0048] 3g of styrene-maleic anhydride was added to water to prepare a styrene-maleic anhydride solution with a mass concentration of 3%, and citric acid was added to adjust the pH to 4-5. The temperature was maintained at 30°C, and 3g of sodium perfluorononyloxybenzenesulfonate was added and stirred to disperse evenly.

[0049] 80 g of perfluorohexanone was added to the above emulsion and dispersed at high speed for 10 min to obtain a mixed emulsion;

[0050] 20g of melamine resin prepolymer was added to the mixed emulsified solution, citric acid was added to adjust the pH of the system to 4-5, and the reaction was carried out for 3h; then 20g of methyl methacrylate was added and the reaction was continued for another 5h to obtain a microcapsule emulsion;

[0051] The microcapsule emulsion was sieved and dried at 40-50° C. for 12 h to obtain fireproof microcapsules with a particle size of 60-120 μm.

[0052] The schematic diagram of the principle of combining fireproof microcapsules with silicone oil in this application is shown in Figure 1 .

[0053] The fireproof microcapsule fire extinguishing tablet and its preparation method provided by the present application are described in detail below with reference to the embodiments and comparative examples.

[0054] Example 1:

[0055] (1) By weight, 70 parts of a bi-terminal vinyl silicone oil with a viscosity of 3500 mPa·s, 20 parts of a side-terminal vinyl silicone oil with a viscosity of 600 mPa·s, 50 parts of a vinyl MQ resin with an M / Q ratio of 0.9, and 0.024 parts of ethynyl cyclohexanol were added to a reaction kettle, and stirred at room temperature for 8 minutes at a speed of 50 r / min until uniformly dispersed to obtain a first mixture;

[0056] (2) adding 7.7 parts by mass of hydrogenated silicone oil having a viscosity of 500 mPa·s and a hydrogen content of 0.8%, 1 part of hydrophobic silica, 2.4 parts of orange paste, and 0.8 parts of yellow paste to the first mixture, stirring at room temperature for 6 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a second mixture;

[0057] (3) while continuing to stir, 0.4 parts by mass of chloroplatinic acid-divinyltetramethyldisiloxane was added to the second mixture, and stirred at room temperature for 10 minutes at a speed of 50 r / min until the mixture was evenly dispersed to obtain a third mixture;

[0058] (4) Add 230 parts by mass of fireproof microcapsules to the third mixture, stir at room temperature for 5 minutes, rotate at 50 r / min, and disperse evenly. Vacuum degassing the obtained rubber material for 1 hour, stop stirring, and discharge the rubber material;

[0059] (5) Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60 ° C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60 ° C drying tunnel, cure for 30 minutes, move out of the drying tunnel, demould, and obtain the fire extinguishing sheet product.

[0060] In Example 1, the fireproof microcapsules were prepared by the following process:

[0061] 30 g of melamine and 60 g of a 37% formaldehyde aqueous solution were added to a three-necked flask, triethanolamine was added dropwise to adjust the pH to 8.5, and the mixture was heated to 85°C in a water bath. The mixture was stirred for 1.5 hours and then discharged to obtain a colorless, clear, and transparent melamine resin prepolymer.

[0062] 3g of styrene-maleic anhydride was added to water to prepare a styrene-maleic anhydride solution with a mass concentration of 3%, and citric acid was added to adjust the pH to 4.5. The temperature was maintained at 30°C, and 3g of sodium perfluorononyloxybenzenesulfonate was added and stirred to disperse evenly.

[0063] 80 g of perfluorohexanone was added to the above emulsion and dispersed at high speed for 10 min to obtain a mixed emulsion;

[0064] 20g of melamine resin prepolymer was added to the mixed emulsified solution, citric acid was added to adjust the system pH to 4, and the mixture was reacted for 3h; then 20g of methyl methacrylate was added and the mixture was reacted for another 5h to obtain a microcapsule emulsion;

[0065] The microcapsule emulsion was sieved and dried at 40°C for 12 h to obtain fireproof microcapsules with a particle size of 80 μm.

[0066] The fire extinguishing tablet product prepared in Example 1 was subjected to performance testing. The specific testing method is as follows:

[0067] 1. Appearance: visual inspection.

[0068] 2. Tensile strength: Tested according to GB / T 528-2009 "Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties".

[0069] 3. Elongation at break: Tested according to GB / T 528-2009 “Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties”.

[0070] 4. Fire extinguishing agent release: Place fire extinguishing tablets of equal mass in an oven at 60℃, 100℃, and 140℃, keep warm for 10 minutes, take out the fire extinguishing tablets and test their mass. Calculate the percentage of mass loss, which is the amount of fire extinguishing agent released at different temperatures.

[0071] 5. Fire extinguishing performance: stick a fire extinguishing sheet of a certain size on the top of the fire extinguishing box, light a flame at the bottom of the fire extinguishing box, and record the time when the flame is completely extinguished.

[0072] 6. Aging performance: Place a certain mass of fire extinguishing tablets in an oven at 60°C for 30 days and calculate their mass loss rate.

[0073] 7. Corrosion performance: Place a small piece of fire extinguishing tablet and a small piece of iron sheet in the same box, open a small hole on the top of the box, place the box in an aging box at 60℃ and 90% RH for 7 days, take it out and check the corrosion of the iron sheet.

[0074] The above test results are shown in Table 1.

[0075] Example 2:

[0076] (1) By weight, 80 parts of a bi-terminal vinyl silicone oil with a viscosity of 6000 mPa·s, 10 parts of a side-terminal vinyl silicone oil with a viscosity of 300 mPa·s, 50 parts of a vinyl MQ resin with an M / Q ratio of 0.8, and 0.024 parts of methylpentynol were added to a reaction kettle, and stirred at room temperature for 6 minutes at a speed of 50 r / min to obtain a uniform dispersion to obtain a first mixture;

[0077] (2) adding 7.4 parts by mass of hydrogenated silicone oil having a viscosity of 400 mPa·s and a hydrogen content of 1.0%, 1 part of hydrophobic silica, 2.4 parts of orange paste, and 0.8 parts of yellow paste to the first mixture, stirring at room temperature for 10 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a second mixture;

[0078] (3) while continuing to stir, 0.4 parts by mass of chloroplatinic acid-divinyltetramethyldisiloxane was added to the second mixture, and stirred at room temperature for 8 minutes at a speed of 50 r / min until the mixture was evenly dispersed to obtain a third mixture;

[0079] (4) Add 223 parts by mass of fireproof microcapsules to the third mixture, stir at room temperature for 6 minutes, rotate at 50 r / min, and disperse evenly. Vacuum degassing the obtained rubber material for 1 hour, stop stirring, and discharge the rubber material;

[0080] (5) Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60 ° C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60 ° C drying tunnel, cure for 30 minutes, move out of the drying tunnel, demould, and obtain the fire extinguishing sheet product.

[0081] The fireproof microcapsules used in Example 2 are the same as those used in Example 1.

[0082] The fire extinguishing tablet product prepared in Example 2 was subjected to performance testing, and the results are shown in Table 1.

[0083] Example 3:

[0084] (1) By weight, 75 parts of a double-end vinyl silicone oil with a viscosity of 1000 mPa·s, 20 parts of a side-end vinyl silicone oil with a viscosity of 1200 mPa·s, 30 parts of a vinyl MQ resin with an M / Q ratio of 1.2, and 0.024 parts of ethynyl cyclohexanol were added to a reaction kettle, and stirred at room temperature for 6 minutes at a speed of 50 r / min to obtain a uniform dispersion to obtain a first mixture;

[0085] (2) adding 7.9 parts by mass of hydrogenated silicone oil having a viscosity of 800 mPa·s and a hydrogen content of 0.9%, 0.5 parts of hydrophobic silica, 2.4 parts of orange paste, and 0.8 parts of yellow paste to the first mixture, stirring at room temperature for 8 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a second mixture;

[0086] (3) while continuing to stir, 0.45 parts by mass of chloroplatinic acid-divinyltetramethyldisiloxane was added to the second mixture, and stirred at room temperature for 6 minutes at a speed of 50 r / min until the mixture was evenly dispersed to obtain a third mixture;

[0087] (4) Add 233 parts by mass of fireproof microcapsules to the third mixture, stir at room temperature for 10 minutes, rotate at 50 r / min, and disperse evenly. Vacuum degassing the obtained rubber material for 1 hour, stop stirring, and discharge the rubber material;

[0088] (5) Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60 ° C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60 ° C drying tunnel, cure for 30 minutes, move out of the drying tunnel, demould, and obtain the fire extinguishing sheet product.

[0089] The fireproof microcapsules used in Example 3 are the same as those used in Example 1. The fire extinguishing tablet product prepared in Example 3 was subjected to performance tests, and the results are shown in Table 1.

[0090] Comparative Example 1:

[0091] (1) adding 100 parts by mass of a double-end vinyl silicone oil with a viscosity of 3500 mPa·s, 40 parts of a side-end vinyl silicone oil with a viscosity of 600 mPa·s, and 0.024 parts of ethynyl cyclohexanol to a reaction kettle, stirring at room temperature for 8 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a first mixture;

[0092] (2) adding 7.2 parts by mass of hydrogenated silicone oil having a viscosity of 500 mPa·s and a hydrogen content of 0.8%, 1 part of hydrophobic silica, 2.4 parts of orange paste, and 0.8 parts of yellow paste to the first mixture, stirring at room temperature for 6 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a second mixture;

[0093] (3) while continuing to stir, add 0.4 parts by mass of chloroplatinic acid-divinyltetramethyldisiloxane to the second mixture, and stir at room temperature for 10 minutes at a speed of 50 r / min until the mixture is evenly dispersed to obtain a third mixture;

[0094] (4) Add 230 parts by mass of fireproof microcapsules to the third mixture, stir at room temperature for 5 minutes, rotate at 50 r / min, and disperse evenly; vacuum degas the evenly dispersed rubber for 1 hour, stop stirring, and discharge the rubber;

[0095] (5) Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60 ° C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60 ° C drying tunnel, cure for 30 minutes, move out of the drying tunnel, demould, and obtain the fire extinguishing sheet product.

[0096] The fireproof microcapsules used in Comparative Example 1 are the same as those used in Example 1. The fire extinguishing tablet product prepared in Comparative Example 1 was subjected to performance tests, and the results are shown in Table 1.

[0097] Comparative Example 2:

[0098] (1) adding 90 parts by mass of a vinyl end-side silicone oil having a viscosity of 600 mPa·s, 50 parts of a vinyl MQ resin having an M / Q ratio of 0.9, and 0.024 parts of ethynyl cyclohexanol to a reaction kettle, stirring at room temperature for 8 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a first mixture;

[0099] (2) adding 8.7 parts by mass of hydrogenated silicone oil having a viscosity of 500 mPa·s and a hydrogen content of 0.8%, 1 part of hydrophobic silica, 2.4 parts of orange paste, and 0.8 parts of yellow paste to the first mixture, stirring at room temperature for 6 minutes at a speed of 50 r / min until uniformly dispersed, to obtain a second mixture;

[0100] (3) while continuing to stir, 0.4 parts by mass of chloroplatinic acid-divinyltetramethyldisiloxane was added to the second mixture, and stirred at room temperature for 10 minutes at a speed of 50 r / min until the mixture was evenly dispersed to obtain a third mixture;

[0101] (4) Add 230 parts by mass of fireproof microcapsules to the third mixture, stir at room temperature for 5 minutes, rotate at 50 r / min, and disperse evenly; vacuum degas the evenly dispersed rubber for 1 hour, stop stirring, and discharge the rubber;

[0102] (5) Move the rubber material to the gluing area of the calender, try to avoid the entry of bubbles during the process, set the drying temperature of the calender to 60 ° C, adjust the distance between the upper and lower rollers of the calender to 2 mm, start the calender, move the rubber material to the 60 ° C drying tunnel, cure for 30 minutes, move out of the drying tunnel, demould, and obtain the fire extinguishing sheet product.

[0103] The fireproof microcapsules used in Comparative Example 2 are the same as those used in Example 1.

[0104] The fire extinguishing tablet product prepared in Comparative Example 2 was subjected to performance testing, and the results are shown in Table 1.

[0105] Comparative Example 3:

[0106] The only difference between Comparative Example 3 and Example 1 is that methyl methacrylate is not added during the preparation of the fireproof microcapsules used in Comparative Example 3; the rest is basically the same as Example 1.

[0107] The fire extinguishing tablet product prepared in Comparative Example 3 was subjected to performance testing, and the results are shown in Table 1.

[0108] Table 1: Test results of fire extinguishing tablets of Examples 1-3 and Comparative Examples 1-3

[0109]

[0110]

[0111] From the data of Example 1 and Comparative Example 1 in Table 1, it can be seen that the tensile strength of the fire extinguishing sheet without the addition of MQ resin is relatively low. The applicant has analyzed that the addition of MQ resin can improve the strength of the fire extinguishing sheet.

[0112] From the data of Example 1 and Comparative Example 2 in Table 1, it can be seen that the tensile strength and elongation at break of the fire extinguishing sheet without the addition of double-ended vinyl silicone oil are relatively low. The applicant analyzed that the tensile strength and elongation at break of the fire extinguishing sheet can be improved by adding double-ended vinyl silicone oil.

[0113] From the data of Example 1 and Comparative Example 3 in Table 1, it can be seen that the fire extinguishing sheet finally obtained by using the fire-resistant microcapsules without adding the active modifier has low tensile strength and elongation at break, poor aging performance, and severe corrosion to the iron sheet. The applicant analyzed that this is because the surface of the fire-resistant microcapsules with the addition of the active modifier contains a large number of active vinyl groups. When added to the organic silica gel water, under the action of the platinum catalyst, the active vinyl groups on the surface of the microcapsules will undergo a silylation reaction with the hydrogen-containing silicone oil, so that the microcapsules and the organic silica gel water have good compatibility, avoiding problems such as phase separation. The microcapsules have good chemical bonding with the glue, effectively improving the fire extinguishing performance and mechanical properties of the fire extinguishing sheet.

[0114] In summary, the fire extinguishing sheet prepared in the examples of the present application exhibits excellent tensile strength and elongation at break.

[0115] In the description of this specification, the description with reference to the terms "one embodiment / method", "some embodiments / methods", "example", "specific example" or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment / method or example are included in at least one embodiment / method or example of the present application. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment / method or example. Moreover, the specific features, structures, materials or characteristics described may be combined in an appropriate manner in any one or more embodiments / methods or examples. In addition, those skilled in the art may combine and combine different embodiments / methods or examples described in this specification and the features of different embodiments / methods or examples, unless they are contradictory.

[0116] It should be noted that, in the present application, relational terms such as "first" and "second" are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply the existence of any such actual relationship or order between these entities or operations. Moreover, the terms "comprise", "include" or any other variants thereof are intended to cover non-exclusive inclusion, so that the process, method, article or equipment comprising a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such process, method, article or equipment. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the presence of other identical elements in the process, method, article or equipment comprising the elements. In the present application, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly specified.

[0117] The foregoing is merely a list of specific embodiments of the present application, intended to enable those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application is not limited to the embodiments shown herein, but is intended to conform to the broadest scope consistent with the principles and novel features of the present application.

Claims

1. A tough organic silicon fireproof microcapsule fire extinguishing sheet, characterized in that: The fire extinguishing sheet includes the following raw materials in parts by mass: 50-80 parts of double-ended vinyl silicone oil, 10-40 parts of end-side vinyl silicone oil, 30-80 parts of reinforcing resin, 1-10 parts of hydrogen-containing silicone oil, 0.2-0.6 parts of platinum catalyst, 0.01-0.04 parts of inhibitor, 0.5-5 parts of reinforcing filler, 1-5 parts of pigment, and 200-300 parts of fireproof microcapsules.

2. The tough organic silicon fireproof microcapsule fire extinguishing sheet according to claim 1, characterized in that: The fireproof microcapsule comprises a core material and a shell material coated on the core material; wherein the core material is a perfluorinated fire extinguishing agent, and the shell material is a non-porous polymer containing an active modifier.

3. The tough organic silicon fireproof microcapsule fire extinguishing sheet according to claim 2, characterized in that: The perfluorinated fire extinguishing agent is a mixture of one or more of perfluorohexanone, perfluorotriethylamine, tetrafluorodibromoethane, difluoromonobromochloromethane, difluorodichloroethane, difluorotrichloroethane, 2-iodo-heptafluoropropane, 1-iodo-heptafluoropropane, and trifluorotrichloroethane; the active modifier is at least one of vinyl monomers or polymers, acrylic acid, methacrylic acid, acrylate, acrylic acid-modified polyurethane, and acrylic acid-modified silicone resin.

4. The tough organic silicon fireproof microcapsule fire extinguishing sheet according to claim 1, characterized in that: The vinyl groups of the double-ended vinyl silicone oil are located at both ends of the silicone oil long chain, and the viscosity at 25°C is 500-10000 mPa·s; the vinyl groups of the side-terminated vinyl silicone oil are located at both ends and side chains of the silicone oil long chain, and the viscosity at 25°C is 100-2000 mPa·s; the viscosity of the hydrogen-containing silicone oil is 100-2000 mPa·s, and the hydrogen content is 0.6%-1.6%; the reinforcing resin is an MQ resin containing vinyl groups, and the M / Q ratio is 0.8-1.

2.

5. The tough organic silicon fireproof microcapsule fire extinguishing sheet according to claim 1, characterized in that: The platinum catalyst is a mixture of any one or more of chloroplatinic acid-divinyltetramethyldisiloxane, chloroplatinic acid-isopropyl alcohol, and chloroplatinic acid-diethyl phthalate; the inhibitor is a mixture of any one or more of methylacetylene alcohol, methylbutynol, methylpentynol, and ethynylcyclohexanol; the reinforcing filler is hydrophobic silica; and the pigment is an oily orange paste or a yellow paste.

6. A method for preparing the tough organic silicon fireproof microcapsule fire extinguishing sheet according to any one of claims 1 to 5, characterized in that: The following steps are involved: S101, mixing bi-terminal vinyl silicone oil, side-terminal vinyl silicone oil, reinforcing resin, and inhibitor, and stirring at room temperature to obtain a first mixture; S102, adding hydrogen-containing silicone oil, reinforcing filler, and pigment to the first mixture, stirring at room temperature to obtain a second mixture; S103, adding the platinum catalyst to the second mixture while stirring, and stirring at room temperature to obtain a third mixture; S104, adding the fireproof microcapsules to the third mixture, stirring at room temperature to obtain a rubber material; vacuum degassing the rubber material and discharging the rubber material; S105, calendering and demolding the rubber material after vacuum degassing and disassembly to obtain the tough organic silicon fireproof microcapsule fire extinguishing sheet.

7. The method for preparing the tough organic silicon fireproof microcapsule fire extinguishing tablet according to claim 6, characterized in that: The fireproof microcapsules are prepared by the following process: adding a perfluorinated fire extinguishing agent to an emulsifier solution, then adding a shell material prepolymer, adding citric acid to adjust the pH value, and then adding an active modifier to react to obtain a microcapsule emulsion; The microcapsule emulsion is sieved and dried to obtain the fireproof microcapsules.

8. The method for preparing the tough organic silicon fireproof microcapsule fire extinguishing tablet according to claim 7, characterized in that: The fireproof microcapsules are specifically prepared by the following process: S201, mixing melamine and formaldehyde aqueous solution, adding triethanolamine to adjust the pH value, heating in a water bath, and stirring to obtain a shell material prepolymer; S202, adding citric acid to the styrene-maleic anhydride solution to adjust the pH, then adding sodium perfluorononyloxybenzenesulfonate, stirring and dispersing uniformly to obtain an emulsifier solution; S203, adding a perfluorinated fire extinguishing agent to the emulsifier solution, dispersing the mixture, and obtaining a mixed emulsion; S204, adding the shell material prepolymer to the mixed emulsion, adding citric acid to adjust the pH value, and then adding an active modifier to react to obtain a microcapsule emulsion; S205, sieving the microcapsule emulsion and drying it to obtain the fireproof microcapsules.

9. The method for preparing the tough organic silicon fireproof microcapsule fire extinguishing tablet according to claim 8, characterized in that: In step S201, triethanolamine is added to adjust the pH value to 8-9, and the temperature of water bath heating is 70-90° C.; in step S202, citric acid is added to adjust the pH value to 4-5.

10. The method for preparing the tough organic silicon fireproof microcapsule fire extinguishing tablet according to claim 9, characterized in that: In step S204, citric acid is added to adjust the pH value to 4-5; in step S205, the drying temperature is 40-50°C.

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