In-situ flame-retardant and fire-extinguishing patch and preparation method thereof
By using high-content flame-retardant fire-extinguishing microcapsules and melamine resins in the patch, the problem of the lack of flame-retardant characteristics of microcapsules shell materials in the prior art is solved, and efficient and rapid fire-extinguishing effect and hardness improvement are achieved, ensuring that Effective fire control in limited confined spaces.
Patent Information
- Application Number
- CN202411362256.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-01-03
AI Technical Summary
The shell materials of existing halogenated hydrocarbon fire extinguishing agent microcapsules lack flame retardant properties, resulting in insufficient flame retardant performance in limited confined spaces, making it difficult to effectively control the initial fire situation.
Using 50-75 wt% flame retardant and fire-extinguishing microcapsules and melamine resins, the explosion temperature and binding force of the microcapsules are improved, and the original with high compressive resistance and rapid fire-extinguishing performance is prepared. Flame-retardant fire-extinguishing patch.
It improves the fire extinguishing efficiency, avoids the reduction of the flame retardant performance of the patch after multiple fire extinguishing, shortens the fire extinguishing time, and enhances the hardness and pressure resistance of the patch, ensuring effective fire control in a limited confined space.
Smart Images
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of fire extinguishing agents, in particular to the field of IPCA62D1, and more specifically to an in-situ flame retardant fire extinguishing patch and a preparation method thereof. Background Art
[0002] Halogenated hydrocarbon fire extinguishing agents have the advantages of low toxicity, fast fire extinguishing speed, no pollution to the environment and no damage to the affected objects, and are widely used in various important places. However, due to the volatility of halogenated hydrocarbons and other fire extinguishing agents, their storage is very difficult. In addition, the supporting equipment for the use of most halogenated hydrocarbons is relatively complex and expensive, which limits their wide application in real life. With the development of microcapsule technology, halogenated hydrocarbon fire extinguishing agents are encapsulated in small microspheres to isolate the air. Since the shell material has a certain strength, the fire extinguishing agent will only be released from the inside of the microsphere when the external temperature reaches a certain value, thereby achieving a fire extinguishing effect.
[0003] Chinese invention patent CN107537127 A discloses a fire extinguishing agent microcapsule patch and its preparation method. Its fire extinguishing principle is to release fire extinguishing gas through the reaction of oxidant and reductant, thereby achieving the purpose of fire extinguishing. However, since the shell material of its fire extinguishing agent microcapsule is methyl methacrylate or polysiloxane material, it does not have flame retardant properties, which greatly weakens the flame retardant properties of the patch. In-situ flame retardant fire extinguishing patches are mainly used to control the initial fire in a limited confined space. How to make the patch into an in-situ flame retardant patch will undoubtedly greatly improve its fire extinguishing efficiency. Summary of the invention
[0004] The first aspect of the present invention provides an in-situ flame retardant and fire extinguishing patch, and the preparation materials include: flame retardant and fire extinguishing microcapsules and matrix resin.
[0005] The content of the flame retardant and fire extinguishing microcapsules in the patch is 50-75wt%.
[0006] Preferably, the content of the flame retardant and fire extinguishing microcapsules in the patch is 60-70wt%.
[0007] Further preferably, the content of the flame retardant and fire extinguishing microcapsules in the patch is 65-70wt%.
[0008] The matrix resin includes one of melamine resin, acrylic resin and silicone resin.
[0009] Preferably, the matrix resin comprises melamine resin.
[0010] The bursting temperature of the flame retardant and fire extinguishing microcapsules is 60-220°C.
[0011] Preferably, the bursting temperature of the flame retardant and fire extinguishing microcapsules is 180-220°C.
[0012] Further preferably, the flame retardant and fire extinguishing microcapsules are prepared with reference to the invention patent CN 115463372 B of the company, and the preferred model is IS-FEM-4.
[0013] The raw materials for preparing the melamine resin include melamine, urea and formaldehyde, and the formaldehyde accounts for 50-80 mol% of the raw materials.
[0014] Preferably, the formaldehyde accounts for 60-80 mol% of the preparation raw materials.
[0015] The raw materials for preparing the acrylic resin include acrylic ester and initiator.
[0016] The raw materials for preparing the organic silicone resin include hydroxy silicone oil, an inorganic precursor and a catalyst.
[0017] The molar ratio of melamine to urea is 1:(1.5-9).
[0018] The present application has found that the content of the flame retardant and fire extinguishing microcapsules in the patch is 50-75wt%, which can avoid the reduction of the flame retardant performance of the patch after multiple fire extinguishing, which may be due to the increase of the fire extinguishing agent released by the rupture of the flame retardant and fire extinguishing microcapsules per unit volume. Further research has found that the molar ratio of melamine and urea is 1: (1.5-9), which can improve the fire extinguishing performance and shorten the fire extinguishing time. On the one hand, it may be due to the increase of the dispersibility of the flame retardant and fire extinguishing microcapsules and the matrix resin, and the improvement of the bonding force between the two, and on the other hand, the improvement of the hardness, thereby improving the pressure resistance of the flame retardant and fire extinguishing microcapsules, so that the capsules can be concentrated in a short time to explode, thereby improving the fire extinguishing performance.
[0019] Preferably, the molar ratio of melamine to urea is 1:(3-7).
[0020] More preferably, the molar ratio of melamine to urea is 1:(5-7).
[0021] The second aspect of the present invention provides a method for preparing an in-situ flame retardant and fire extinguishing patch, comprising the following steps:
[0022] S1, preparing flame retardant and fire extinguishing microcapsules;
[0023] S2, preparing base resin;
[0024] S3, adding the flame retardant and fire extinguishing microcapsules into the base resin, adjusting the pH value to 1-4, and stirring evenly to obtain a mixture;
[0025] S4, pouring the mixture into a mold and baking and curing the mixture.
[0026] The baking time is 6-10 hours.
[0027] Preferably, the baking time is 6-10 hours.
[0028] The base resin is melamine resin, and step S2 specifically comprises the following steps: adding melamine, urea and formaldehyde, adjusting the pH value to 8-9 with alkaline solution, stirring and dissolving, stirring at 60-90° C. for 1-2 hours, and cooling to obtain the product.
[0029] The base resin is melamine resin, and step S3 specifically includes the following steps: adding hydrochloric acid to the base resin to adjust the pH value to 2-3, then slowly adding component A to component B within 10-30 minutes, adding while stirring with a glass rod, and fully mixing to obtain a mixture.
[0030] The base resin is an organic silicon resin, and step S2 specifically comprises the following steps: adding hydroxy silicone oil, an inorganic precursor, and a catalyst, mixing them thoroughly and uniformly, and cooling them to obtain the result.
[0031] The base resin is acrylic resin, and step S2 specifically comprises the following steps: adding acrylic ester and initiator, mixing them thoroughly and uniformly, and cooling them to obtain the product.
[0032] The base resin is silicone resin or acrylic resin, and step S1 also includes adding a flame retardant.
[0033] Beneficial Effects
[0034] 1. Selecting flame retardant fire extinguishing microcapsules with a bursting temperature of 60-220℃ can improve the fire extinguishing efficiency.
[0035] 2. Melamine resin is selected as the base resin, and no additional flame retardant is needed. At the same time, the occurrence of re-ignition after flame retardancy can be avoided.
[0036] 3. The content of the flame retardant and fire extinguishing microcapsules in the patch is 50-75wt%, which can prevent the flame retardant performance of the patch from decreasing after multiple fire extinguishing.
[0037] 4. The molar ratio of melamine to urea is 1:(1.5-9), which can further improve the fire extinguishing performance and shorten the fire extinguishing time, so that it can be used to control the initial fire in a limited confined space.
[0038] 5. The in-situ flame retardant and fire extinguishing patch of this application can be prepared quickly, with simple process and convenient operation. BRIEF DESCRIPTION OF THE DRAWINGS
[0039] Figure 1 This is an electron microscope image of the flame retardant and fire extinguishing microcapsules in Example 1.
[0040] Figure 2This is a physical picture of the patch prepared in Example 1.
[0041] Figure 3 This is a photo of the patch prepared in Example 1 after testing. DETAILED DESCRIPTION
[0042] Example 1
[0043] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0044] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0045] (1) Configuration of flame retardant and fire extinguishing microcapsules: Use a 100 mL beaker to weigh 60 parts (by weight) of fire extinguishing microcapsule powder IS-FEM-2 (produced by our company, the capsule bursting temperature is 80-100°C, the electron microscope image is as follows Figure 1 As shown), it is component A and is for standby use.
[0046] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 4 g melamine, 12 g urea, and 50 g 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0047] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then slowly add component A to component B within 20 minutes, stir with a glass rod, and mix thoroughly to obtain glue solution C.
[0048] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h to obtain the following: Figure 2 Patch shown.
[0049] Example 2
[0050] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0051] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0052] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 60 parts by weight of fire extinguishing microcapsule powder IS-FEM-4 (produced by our company, with a capsule bursting temperature of 200-220°C) in a 100 mL beaker as component A and set aside.
[0053] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 4 g melamine, 12 g urea, and 50 g 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0054] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then slowly add component A to component B within 20 minutes, stir with a glass rod, and mix thoroughly to obtain glue solution C.
[0055] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0056] Example 3
[0057] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0058] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0059] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 60 parts by weight of fire extinguishing microcapsule powder IS-FEM-4 (produced by our company, with a capsule bursting temperature of 200-220°C) in a 100 mL beaker as component A and set aside.
[0060] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 5 g of melamine, 11 g of urea, and 50 g of 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g of melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0061] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then add 10 g of 5 % PVA solution, and then slowly add component A to component B within 20 min, stirring with a glass rod, and mix thoroughly to obtain glue solution C.
[0062] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0063] Example 4
[0064] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0065] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0066] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 60 parts by weight of fire extinguishing microcapsule powder IS-FEM-4 (produced by our company, with a capsule bursting temperature of 200-220°C) in a 100 mL beaker as component A and set aside.
[0067] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 6 g of melamine, 10 g of urea, and 50 g of 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g of melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0068] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then slowly add component A to component B within 20 minutes, stir with a glass rod, and mix thoroughly to obtain glue solution C.
[0069] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0070] Example 5
[0071] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0072] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0073] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 65 parts of fire extinguishing microcapsule powder IS-FEM-4 (produced by our company, with a capsule bursting temperature of 200-220°C) in a 100 mL beaker as component A and set aside.
[0074] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 6 g of melamine, 10 g of urea, and 50 g of 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g of melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0075] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then slowly add component A to component B within 20 minutes, stir with a glass rod, and mix thoroughly to obtain glue solution C.
[0076] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0077] Example 6
[0078] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and melamine resin.
[0079] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0080] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 70 parts of fire extinguishing microcapsule powder IS-FEM-4 (produced by our company, with a capsule bursting temperature of 200-220°C) in a 100 mL beaker as component A and set aside.
[0081] (2) Configuration of base resin: Preparation of melamine prepolymer: In a 100 mL glass flask, add 6 g of melamine, 10 g of urea, and 50 g of 37 wt% formaldehyde solution, adjust the pH value to 8.5 with 10 wt% NaOH, stir and dissolve, stir at 75°C for 1 h, and obtain 66 g of melamine prepolymer with a solid content of 52.3 wt%. Pour the mixture into a 250 mL beaker and cool for use as component B.
[0082] (3) Add 10 wt % hydrochloric acid to component B to adjust the pH value to 2.5, then slowly add component A to component B within 20 minutes, stir with a glass rod, and mix thoroughly to obtain glue solution C.
[0083] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0084] Comparative Example 1
[0085] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and acrylic resin.
[0086] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0087] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 60 parts (by weight) of fire extinguishing microcapsule powder in a 100 mL beaker, add 10-20 parts of flame retardant thereto, mix thoroughly and evenly to obtain component A for later use.
[0088] (2) Preparation of base resin: In a 100 mL beaker, 20 parts of methyl methacrylate, 2 parts of trimethylolpropane trimethacrylate, and 0.2 g of TPO (trimethylbenzoyl-diphenylphosphine oxide) were weighed in a certain proportion, mixed well, poured into a 250 mL beaker, and cooled for use as component B.
[0089] (3) Slowly add component A to component B, stirring with a glass rod, and mix thoroughly to obtain glue solution C.
[0090] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in an oven at 60°C and bake.
[0091] Comparative Example 2
[0092] An in-situ flame retardant and fire extinguishing patch is prepared from flame retardant and fire extinguishing microcapsules and organic silicon resin.
[0093] An in-situ flame retardant and fire extinguishing patch, the preparation method of which is as follows:
[0094] (1) Preparation of flame retardant and fire extinguishing microcapsules: Weigh 60 parts by weight of fire extinguishing microcapsule powder IS-FEM-2 (produced by our company, with a capsule bursting temperature of 80-100°C) in a 100 mL beaker, add 15 parts of Al(OH) 3 , mix thoroughly and evenly to obtain component A, set aside.
[0095] (2) Preparation of base resin: To prepare the silicone base resin, weigh 300 parts of hydroxy silicone oil, 3 parts of TEOS (tetraethoxysilane), and 0.8 parts of tin laurate T12 (dibutyltin laurate) in a certain proportion in a 100 mL beaker, mix them thoroughly, pour them into a 250 mL beaker, and cool them for later use. This is component B.
[0096] (3) Slowly add component A to component B, stirring with a glass rod, and mix thoroughly to obtain glue solution C.
[0097] (4) Pour C into a square mold with a length, width and height of 200 mm × 100 mm × 30 mm respectively, and vibrate the mold rapidly to allow the mixture to quickly flow to every corner of the mold. Then, place the mold in a 50°C oven and bake for 7 h.
[0098] Performance testing methods and data
[0099] The in-situ flame retardant and fire extinguishing patch prepared in the embodiment was subjected to performance testing with reference to Q31 / 0115001112C001-2019, and the test data are listed in Table 1.
[0100] Table 1
[0101]
[0102]
[0103] like Figure 3 As shown, the patch of Example 1 did not change significantly after the test and had excellent flame retardant effect. By comparing the schemes of Examples 1-2 and Comparative Example 1-2, it can be seen that the microspheres prepared using melamine patches have a higher fire extinguishing efficiency, and the capsule IS-FEM-4 has a higher fire extinguishing efficiency than IS-FEM-2. Comparing the schemes of Examples 3-6, under the same capsule content, the harder the hardness of the obtained patch, the better the fire extinguishing performance of the patch, and the higher the efficiency. As the amount of capsule added increases, the hardness of the patch increases, and the fire extinguishing efficiency also increases slightly. In summary, a fire extinguishing patch with high fire extinguishing efficiency is prepared by adjusting the hardness of the patch.
Claims
1. An in-situ flame retardant fire extinguishing patch, characterized in that: The preparation raw materials include: flame retardant and fire extinguishing microcapsules and base resin.
2. The in-situ flame retardant and fire extinguishing patch according to claim 1, characterized in that: The content of the flame retardant and fire extinguishing microcapsules in the patch is 50-75wt%.
3. The in-situ flame retardant and fire extinguishing patch according to claim 2, characterized in that: The matrix resin includes one of melamine resin, acrylic resin and silicone resin.
4. The in-situ flame retardant and fire extinguishing patch according to claim 3, characterized in that: The bursting temperature of the flame retardant and fire extinguishing microcapsules is 60-220°C.
5. The in-situ flame retardant and fire extinguishing patch according to claim 1 or 4, characterized in that: The bursting temperature of the flame retardant and fire extinguishing microcapsules is 180-220°C.
6. The in-situ flame retardant and fire extinguishing patch according to claim 2, characterized in that: The raw materials for preparing the melamine resin include melamine, urea and formaldehyde, and the formaldehyde accounts for 50-80 mol% of the raw materials.
7. The in-situ flame retardant and fire extinguishing patch according to claim 6, characterized in that: The molar ratio of melamine to urea is 1:(1.5-9).
8. The in-situ flame retardant and fire extinguishing patch according to claim 7, characterized in that: The molar ratio of melamine to urea is 1:(3-7).
9. A method for preparing the in-situ flame retardant and fire extinguishing patch according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1, preparing flame retardant and fire extinguishing microcapsules; S2, preparing base resin; S3, adding the flame retardant and fire extinguishing microcapsules into the base resin, adjusting the pH value to 1-4, and stirring evenly to obtain a mixture; S4, pouring the mixture into a mold and baking and curing the mixture.
10. The method for preparing the in-situ flame retardant and fire extinguishing patch according to claim 9, characterized in that: The baking time is 6-10 hours.