Novel flame-retardant fire extinguishing material as well as preparation method and application thereof

By preparing a new type of flame-retardant fire-extinguishing material containing specific powder components, the problem of traditional fire extinguishing agents reigniting under long-term flame burning is solved, and the dual effects of rapid extinguishing and flame retardancy are achieved. It is suitable for ordinary water-based fire extinguishing equipment, forest fire prevention and lithium-ion battery flame retardancy.

CN120643871APending Publication Date: 2025-09-16SICHUAN BAIZHONGAN NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202510656405.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-21
Publication Date
2025-09-16

AI Technical Summary

Technical Problem

Existing fire extinguishing agents do not have excellent flame retardant properties under long-term flame burning, causing combustible materials to reignite or burn, and cannot effectively prevent the spread of flames, posing a safety hazard, especially in ancient buildings and forest fires.

Method used

A new type of flame retardant fire extinguishing material is used, which includes potassium, sodium, calcium, magnesium, iron, aluminum oxide silicate powder, silicate mineral powder, chemically modified graphite powder and insoluble bicarbonate powder. The mixed solution prepared by a specific process has good stability, fluidity, adhesion and flame retardant properties.

Benefits of technology

It achieves the dual effects of fire extinguishing and flame retardancy, can quickly extinguish fires and prevent re-ignition, has excellent flame retardant properties and heat absorption, the material is non-toxic and non-corrosive, the site preparation is simple, it protects equipment and facilities, and its heat absorption far exceeds that of traditional fire extinguishing materials.

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Abstract

The invention discloses a novel flame-retardant fire extinguishing material and a preparation method and application thereof, and belongs to the field of flame retardance and fire fighting, and the material comprises the following components in parts by weight: 5-30 parts of raw material heat treatment powder, 100-200 parts of a dispersion medium, 0.5-1.25 parts of a dispersion medium auxiliary agent, 0.6-0.8 part of polyamide, 1.25-2.5 parts of a thickening agent and 0.2-0.5 part of a preservative. The fire retardant has a good flame retardant effect and a good fire extinguishing effect in the fire extinguishing process, and generation of toxic smoke can be greatly reduced.
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Description

Technical Field

[0001] The present invention relates to the field of flame retardant firefighting, and in particular to a novel flame retardant fire extinguishing material, a preparation method and application thereof. Background Art

[0002] The various types of existing fire extinguishing materials have their own characteristics and advantages, and can effectively extinguish and suppress fires of types A, B, C, D, E, and F. For example, foam fire extinguishing agents have multiple functions during the fire extinguishing process, including covering, isolating, cooling, and diluting, and can extinguish Class A and B fires. Dry powder fire extinguishing agents have suffocating, cooling, and chemically inhibiting combustion effects, and can extinguish Class A, B, C, D, and E fires. However, the traditional types of fire extinguishing agents we commonly see do not have excellent flame retardant properties. Even after covering, if the flame burns for a long time, it will still cause the combustible materials to reignite or burn, ultimately leading to the collapse of ancient buildings, injuries or even deaths of firefighters, or the rapid and uncontrolled spread of forest fires. Therefore, it is necessary to develop a new type of fire extinguishing material with excellent fire extinguishing and flame retardant properties to meet the needs of fire extinguishing in various fire scenarios. Summary of the Invention

[0003] One of the purposes of the present invention is to provide a new type of flame retardant fire extinguishing material to solve the problem that traditional types of fire extinguishing agents in the prior art still do not have excellent flame retardant function.

[0004] The present invention is achieved through the following technical solution. A new flame retardant and fire extinguishing material comprises the following components in parts by weight: 5-30 parts of raw material heat-treated powder, 100-200 parts of dispersion medium, 0.5-1.25 parts of dispersion medium additive, 0.6-0.8 parts of polyamide, 1.25-2.5 parts of thickener, and 0.2-0.5 parts of preservative.

[0005] Furthermore, the raw material heat-treated powder is a combination of one or more of potassium sodium calcium magnesium iron oxide aluminum silicate powder, silicate mineral powder, chemically modified graphite powder and insoluble bicarbonate powder.

[0006] Furthermore, the particle size of the raw material heat-treated powder is 100 to 2000 meshes.

[0007] Furthermore, the active modification groups in the chemically modified graphite powder are a combination of one or more of sulfonic acid groups, stearate groups, sulfate groups and nitro groups.

[0008] On the other hand, the present invention provides a method for preparing a novel flame retardant and fire extinguishing material, comprising the following steps: adding 25 parts of the components described in the novel flame retardant and fire extinguishing material, according to the raw material heat-treated powder, 150 parts of a dispersion medium, and 0.75 parts of a dispersion medium additive, to 150 parts of water, stirring and dispersing to prepare a first mixed solution; adding 0.7 parts of polyamide and 2 parts of a thickener to the first mixed solution, stirring and dispersing to prepare a second mixed solution; adding 0.25 parts of a post-preservative to the second mixed solution, and adjusting the pH of the second mixed solution to 7.5 using a NaH2PO4 / Na2HPO4 solution.

[0009] Furthermore, the raw material heat-treated powder is an insoluble bicarbonate powder, which is prepared by hydrolyzing and polycondensing TEOS (tetraethyl orthosilicate) sol to generate a silicon dioxide network coating layer.

[0010] Furthermore, the hydrolysis-polycondensation reaction of TEOS sol to generate a silica network coating layer includes the following steps: preparing a mixed precursor solution with a molar ratio of TEOS:EtOH:H2O=1:4:8; adding NH3·H2O as a catalyst to the mixed precursor solution, and adjusting the pH to 8-10 to prepare a third mixed solution; stirring the third mixed solution in a 50-70°C water bath at 300-500 rpm using a magnetic stirrer for 1-3 hours, and then stopping heating to complete the key reaction; after stopping heating, continuing stirring at room temperature for 6-12 hours to further cross-link the SiO2 nanoparticles to form a stable sol; dispersing sodium bicarbonate powder in the sol, stirring for 1-2 hours to uniformly deposit SiO2, and preparing an insoluble bicarbonate powder coated with SiO2 after filtering and drying.

[0011] Furthermore, the reaction formula of the key reaction is:

[0012]

[0013] Furthermore, the raw material heat-treated powder is an insoluble bicarbonate powder, and the insoluble bicarbonate powder is prepared by generating a silicon dioxide network coating layer through a hydrolysis-polycondensation reaction of TEOS sol.

[0014] Furthermore, the raw material heat-treated powder is chemically modified graphite powder.

[0015] Furthermore, the chemically modified denatured graphite powder is prepared by the following steps: according to the weight ratio of graphite: acetic anhydride: HNO3: potassium permanganate of 1:0.5-1:0.2-0.7:0.03-0.1, acetic anhydride and concentrated nitric acid are first added, then potassium permanganate is added, and finally graphite powder is added, stirred, reacted for 40-80 minutes, and then filtered, 30% hydrogen peroxide is added and stirring is continued until the potassium permanganate reaction is completely stopped and no gas is generated, washed with water to pH = 5-7, filtered, and dried at 30-65°C to prepare the chemically modified denatured graphite powder.

[0016] On the other hand, the present invention provides an application of a novel flame retardant fire extinguishing material. The flame retardant fire extinguishing material obtained according to the component ratio of the novel flame retardant fire extinguishing material, or the flame retardant fire extinguishing material prepared according to the novel flame retardant fire extinguishing material has the following applications: (1) application in the preparation of ordinary water-based fire extinguishing equipment; (2) application in forest fire prevention / extinguishing; (3) application in the flame retardancy of lithium-ion batteries.

[0017] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0018] 1. The novel flame retardant and fire extinguishing material of the present invention can be uniformly and stably dispersed in the system for a long time under the condition of weak ion action, achieving mutual coordination and synergy of the components, so that the system has good stability, flowability, adhesion, isolation, flame retardancy, heat absorption, insulation and shearing properties, and finally completes the rapid extinguishing of the fire and can effectively prevent the re-ignition of the fire. After covering the surface of the combustible material, it can effectively prevent the object from being ignited, achieving the dual effects of fire extinguishing and flame retardancy. In addition, the fire extinguishing material is also environmentally friendly and non-toxic and fluorine-free, and the material is non-corrosive. The site preparation is simple and easy to clean, and it can protect various types of equipment and facilities in the fire scene, which is different from traditional flame retardant coatings.

[0019] 2. The novel flame-retardant fire-extinguishing material of the present invention can ensure long-term suspension (>5 years), avoid the occurrence of inhomogeneity, ensure the quality of fire-fighting materials and stable fire-extinguishing effect; at the same time, it has strong flame-retardant properties and has extremely excellent performance in preventing flame combustion and spread, which greatly exceeds traditional fire-extinguishing materials. It can adhere to the surface of the burning object and quickly suppress the fire until the fire is reduced or extinguished, thus quickly extinguishing the fire.

[0020] 3. The new flame retardant fire extinguishing material of the present invention has good heat absorption and can effectively reduce combustion free radicals. Its heat absorption reaches about 1400kJ / kg, which is more than 10 times the heat absorption performance parameter of perfluorohexanone fire extinguishing agent, and the effective utilization rate of the material exceeds that of traditional fire extinguishing materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, constitute a part of this application, and do not constitute a limitation of the embodiments of the present invention. In the drawings:

[0022] Figure 1 Specific heat capacity diagram provided for the experimental examples of the present invention.

[0023] Figure 2 This is a diagram of latent heat of vaporization provided for the experimental examples of the present invention.

[0024] Figure 3 This is a thixotropy diagram provided for the experimental examples of the present invention. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments.

[0026] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this invention pertains. Although preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention. All references mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials to which they relate. In the event of a conflict with any incorporated reference, the present specification controls. As used herein, the terms "including," "comprising," "having," "containing," and the like are open-ended, meaning to include, but not be limited to. Unless the context clearly dictates otherwise, the expressions "a," "an," and "a" include plural references. It should be noted that the terms "first," "second," and the like are used solely for convenience of description and distinction and are not to be construed as indicating or implying relative importance. As used herein, the term "about" refers to a range of ±20% of the value that follows it. In some embodiments, the term "about" refers to a range of ±10% of the value that follows it. In some embodiments, the term "about" refers to a range of ±5% of the value that follows it.

[0027] Example 1

[0028] This embodiment discloses a novel flame retardant and fire extinguishing material, comprising the following components in parts by weight:

[0029] 5 parts of raw material heat-treated powder, 100 parts of dispersion medium, 0.5 parts of dispersion medium additive, 0.6 parts of polyamide, 1.25 parts of thickener, and 0.2 parts of preservative.

[0030] The raw material heat-treated powder in this embodiment is potassium sodium calcium magnesium iron oxide aluminum silicate powder, and its particle size is 100 mesh.

[0031] The preparation steps include: adding 5 parts of raw material heat-treated powder, 100 parts of dispersion medium, and 0.5 parts of dispersion medium additive to 150 parts of water, and stirring and dispersing for 30 minutes to prepare a first mixed solution.

[0032] Add 0.6 parts of polyamide and 1.25 parts of thickener to the first mixed solution, and stir and disperse for 30 minutes to prepare a second mixed solution;

[0033] 0.2 parts of post-corrosion preservative were added to the second mixed solution, and the pH of the second mixed solution was adjusted to 7.5 using NaH2PO4 / Na2HPO4 solution to obtain the novel flame retardant and fire extinguishing material of this embodiment.

[0034] Example 2

[0035] This embodiment discloses a novel flame retardant and fire extinguishing material, comprising the following components in parts by weight:

[0036] 15 parts of raw material heat-treated powder, 150 parts of dispersion medium, 0.8 parts of dispersion medium additive, 0.7 parts of polyamide, 1.5 parts of thickener, and 0.3 parts of preservative.

[0037] The raw material heat-treated powder in this embodiment is silicate mineral powder, and its particle size is 2000 mesh.

[0038] The preparation steps include: adding 15 parts of raw material heat-treated powder, 150 parts of dispersion medium, and 0.8 parts of dispersion medium additive to 150 parts of water, and stirring and dispersing for 60 minutes to prepare a first mixed solution.

[0039] 0.7 parts of polyamide and 1.5 parts of thickener were added to the first mixed solution, and the mixture was stirred and dispersed for 60 minutes to prepare a second mixed solution.

[0040] 0.3 parts of post-corrosion preservative was added to the second mixed solution, and the pH of the second mixed solution was adjusted to 7.5 using NaH2PO4 / Na2HPO4 solution to obtain the novel flame retardant and fire extinguishing material of this embodiment.

[0041] Example 3

[0042] This embodiment discloses a novel flame retardant and fire extinguishing material, comprising the following components in parts by weight:

[0043] Raw materials: 20 parts of heat-treated powder, 175 parts of dispersion medium, 1.2 parts of dispersion medium additive, 0.8 parts of polyamide, 2 parts of thickener, and 0.5 parts of preservative.

[0044] The raw material heat-treated powder in this embodiment is chemically modified graphite powder, and the particle size of the powder is 500 mesh.

[0045] Specifically, chemically modified graphite powder is prepared by the following sub-steps:

[0046] The weight ratio of graphite: acetic anhydride: HNO3: potassium permanganate is 1:0.5-1:0.2-0.7:0.03-0.1.

[0047] First add acetic anhydride and concentrated nitric acid, then add potassium permanganate, and finally add graphite powder.

[0048] The mixture was stirred and reacted for 40-80 minutes, then filtered and added with 30% hydrogen peroxide, and the stirring was continued until the potassium permanganate reaction was complete and no more gas was generated. The mixture was washed with water until the pH value was 5-7, filtered, and dried at 30-65° C. to prepare the chemically modified graphite powder in this embodiment.

[0049] Then, 20 parts of chemically modified graphite powder, 175 parts of dispersion medium, and 1.2 parts of dispersion medium additive were added to 150 parts of water, and the mixture was stirred and dispersed to prepare a first mixed solution.

[0050] 0.8 parts of polyamide and 2 parts of thickener were added to the first mixed solution, and the mixture was stirred and dispersed to prepare a second mixed solution.

[0051] 0.5 parts of post-corrosion preservative was added to the second mixed solution, and the pH of the second mixed solution was adjusted to 7.5 using NaH2PO4 / Na2HPO4 solution to obtain the novel flame retardant and fire extinguishing material of this embodiment.

[0052] Example 4

[0053] This embodiment discloses a novel flame retardant and fire extinguishing material, which differs from embodiment 3 in that the raw material heat-treated powder in this embodiment is an insoluble bicarbonate powder. The remaining steps are exactly the same as those in embodiment 3.

[0054] Specifically, the insoluble bicarbonate powder is prepared by the following steps:

[0055] The insoluble bicarbonate powder was prepared using a tetraethyl orthosilicate (TEOS) sol method, in which a silica network coating layer was generated by a hydrolysis-polycondensation reaction of TEOS sol.

[0056] 1) Materials and equipment: tetraethyl orthosilicate (TEOS, purity >98%), anhydrous ethanol (EtOH), water, ammonia (25%), a magnetic stirrer, and a constant temperature water bath.

[0057] 2) Operation steps: First prepare a mixed precursor solution, according to the (molar ratio) of TEOS:EtOH:H2O = 1:4:8 (alkaline conditions), add a catalyst (NH3·H2O for alkaline conditions), adjust the pH to 8-10 (base catalysis), and stir (300-500 rpm) in a 50-70°C water bath for 1-3 hours until the solution becomes a transparent sol, completing the key reaction.

[0058] The key reaction equation is:

[0059]

[0060] 3) Stop heating and continue stirring at room temperature for 6-12 hours to further crosslink the SiO2 nanoparticles (typically 5-50 nm) and form a stable sol. 4) Disperse sodium bicarbonate powder in the sol and stir for 1-2 hours to uniformly deposit the SiO2. Finally, filter and dry (50-55°C) to obtain insoluble sodium bicarbonate particles coated with SiO2.

[0061] Experimental Example 1

[0062] The test results of the new flame retardant and fire extinguishing material prepared in Example 3 are shown in Table 1.

[0063] Table 1. Test results

[0064]

[0065] Figure 1 The specific heat capacity diagram of the material obtained through this experiment is shown. Figure 2 The graph shows the latent heat of vaporization of the material obtained through this experiment. Figure 3 The thixotropy diagram of the material obtained through this experiment is shown.

[0066] Experimental Example 2

[0067] The new flame retardant and fire extinguishing material prepared in Example 3 was subjected to a white cardboard flame retardancy test.

[0068] Test conditions: 1. Alcohol lamp holder fixed at the same height; 2. Apply different fire extinguishing materials evenly to the front and back of the card; 3. Secure the coated card to the alcohol lamp holder; 4. Place the alcohol lamp directly below the card; 5. Place a stopwatch on one side of the alcohol lamp holder.

[0069] Experimental operation: 1. Light the alcohol lamp to burn the card and start the timer at the same time. 2. When the card starts burning, stop the timer at the same time. The experimental results are shown in Table 2.

[0070] Table 2. Flame retardant test results of white cardboard

[0071] Serial number Type of fire extinguishing agent Burning time 1 F-5006% 10.5S 2 Water-based foam 10.3S 3 Nanoclusters - 6% 9.2S 4 water 6.7S 5 No medicine 6.3S 6 Example 3 47.1S

[0072] Experimental Example 3

[0073] (1) The new flame retardant and fire extinguishing material prepared in Example 1 was subjected to a long wood strip flame retardancy test.

[0074] After coating long wooden strips (40 mm*40 mm*630 mm) with the novel flame retardant and fire extinguishing material prepared in Example 1, a frame was constructed in the shape of 8*16, and the fire extinguishing object was ignited by igniting 2.0 L of n-heptane.

[0075] (2) For the novel flame-retardant fire-extinguishing material prepared in Example 3, standard 1A model wood strips (40mm*40mm*500mm) were used, in a 12-layer arrangement of 8 strips. The oil pan dimensions were 400mm*400mm*100mm; the oil volume was 1.1L, and the support height was 400mm. A multi-phase fire-extinguishing material and a water-based fire-extinguishing agent were uniformly sprayed onto the surface of the wood strips.

[0076] Table 3. Wood strip flame retardant test results

[0077]

[0078] Experimental Example 4

[0079] Lithium battery fire extinguishing effect experiment: According to the national standard requirements of water-based fire extinguishers, a 6 kg fire extinguisher containing the new flame retardant fire extinguishing material prepared in Example 3 was filled (two 3 kg, Class D fire extinguishers were prepared). The nozzle was connected to a galvanized pipe with a nozzle through a long plastic tube and installed above the test stand for standby use. Use an 18650 battery (48V20AH) and heat it with a cassette stove. When the external temperature is about 680°C, the lithium battery electrolyte begins to spray out and automatically ignite. After 10 minutes, the fire became larger, and the fire extinguisher handle was pressed to extinguish the fire. The experimental results are shown in Table 4.

[0080] Table 4. Lithium battery fire extinguishing effect test table

[0081]

[0082] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A new type of flame retardant fire extinguishing material, characterized in that: The flame retardant fire extinguishing material comprises the following components in parts by weight: 5-30 parts of raw material heat-treated powder, 100-200 parts of dispersion medium, 0.5-1.25 parts of dispersion medium additive, Polyamide 0.6-0.8 parts, Thickener 1.25-2.5 parts, 0.2-0.5 parts of preservatives.

2. The novel flame retardant and fire extinguishing material according to claim 1, characterized in that: The raw material heat-treated powder is a combination of one or more of potassium, sodium, calcium, magnesium, iron, aluminum oxide silicate powder, silicate mineral powder, chemically modified graphite powder and insoluble bicarbonate powder.

3. The novel flame retardant and fire extinguishing material according to claim 1, characterized in that: The particle size of the raw material heat-treated powder is 100 to 2000 meshes.

4. The novel flame retardant and fire extinguishing material according to claim 2, characterized in that: The active modification groups in the chemically modified graphite powder are a combination of one or more of sulfonic acid groups, stearate groups, sulfuric acid groups and nitro groups.

5. A method for preparing a new type of flame retardant and fire extinguishing material, characterized in that: The preparation method comprises: adding 25 parts of the components described in any one of claims 1 to 4, 150 parts of the raw material heat-treated powder, 150 parts of the dispersion medium, and 0.75 parts of the dispersion medium additive to 150 parts of water, and stirring and dispersing to prepare a first mixed solution; Add 0.7 parts of polyamide and 2 parts of thickener to the first mixed solution, stirring and dispersing to prepare a second mixed solution; 0.25 parts of post-preservative was added to the second mixed solution, and the pH of the second mixed solution was adjusted to 7.5 using NaH2PO4 / Na2HPO4 solution.

6. The method for preparing the novel flame retardant and fire extinguishing material according to claim 5, characterized in that: The raw material heat-treated powder is an insoluble bicarbonate powder, The insoluble bicarbonate powder is prepared by generating a silicon dioxide network coating layer through a hydrolysis-polycondensation reaction of TEOS sol.

7. The method for preparing the novel flame retardant and fire extinguishing material according to claim 5, characterized in that: The raw material heat-treated powder is chemically modified graphite powder.

8. The method for preparing the novel flame retardant and fire extinguishing material according to claim 7, characterized in that: The chemically modified graphite powder is prepared by the following steps: The weight ratio of graphite, acetic anhydride, HNO3 and potassium permanganate is 1:0.5-1:0.2-0.7:0.03-0.

1. Acetic anhydride and concentrated nitric acid are first added, followed by potassium permanganate, and finally graphite powder is added. The mixture is stirred, reacted for 40-80 minutes, and then filtered. 30% hydrogen peroxide is added and stirring is continued until the potassium permanganate reaction is complete and no gas is generated. The mixture is washed with water to a pH of 5-7, filtered, and dried at 30-65° C. to prepare chemically modified graphite powder.

9. Application of a new type of flame retardant fire extinguishing material, characterized in that: The novel flame retardant and fire extinguishing material is obtained according to the component ratio described in any one of claims 1 to 4, or is prepared according to the preparation method described in any one of claims 5 to 7. Applications include: (1) Application in the preparation of ordinary water-based fire extinguishing equipment; (2) Application in forest fire prevention / extinguishing; (3) Application in flame retardancy of lithium-ion batteries.