阅读说明：本技术 一种多功能全氟己酮灭火剂及其制备方法 (Multifunctional perfluorohexanone fire extinguishing agent and preparation method thereof ) 是由 沈奂 张祖雄 宫彦齐 于 2021-08-25 设计创作，主要内容包括：本发明提出一种多功能全氟己酮灭火剂,包括水系灭火剂原材料,所述水系灭火剂原材料重量比的制备原料：全氟己酮25-35％、可膨胀石墨12-18％、壳聚糖接枝的聚(丙烯酸-共-甲基丙烯酰胺)水凝胶15-20％和分散剂8-10％,所述壳聚糖接枝的聚(丙烯酸-共-甲基丙烯酰胺)凝胶可延长全氟己酮在火源表面的作用时间,提高灭火剂的灭火效果,且水凝胶可以协同膨胀石墨对火源表面释放的烟雾和毒气进行吸附,得到一种具有优异灭火性能且能吸附烟雾和毒气的灭火剂。(The invention provides a multifunctional perfluorohexanone fire extinguishing agent, which comprises the following raw materials in parts by weight: 25-35% of perfluorohexanone, 12-18% of expandable graphite, 15-20% of chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel and 8-10% of a dispersing agent, wherein the chitosan-grafted poly (acrylic acid-co-methacrylamide) gel can prolong the action time of the perfluorohexanone on the surface of a fire source and improve the fire extinguishing effect of the fire extinguishing agent, and the hydrogel can be used for adsorbing smoke and toxic gas released from the surface of the fire source in a synergistic manner with the expanded graphite to obtain the fire extinguishing agent which has excellent fire extinguishing performance and can adsorb the smoke and the toxic gas.)

1. The multifunctional perfluorohexanone fire extinguishing agent comprises a water-based fire extinguishing agent raw material, and is characterized by also comprising the following preparation raw materials in percentage by weight of the water-based fire extinguishing agent raw material: 25-35% of perfluorohexanone, 12-18% of expandable graphite, 15-20% of chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel and 8-10% of dispersing agent.

2. The multifunctional perfluorohexanone fire extinguishing agent according to claim 1, wherein the expandable graphite is prepared by a method comprising the steps of: and (3) stirring hydrogen peroxide, flake graphite and concentrated nitric acid for reaction, and then washing and drying the obtained reaction product to obtain the expandable graphite.

3. The multifunctional perfluorohexanone fire extinguishing agent according to claim 2, wherein the mass ratio of hydrogen peroxide, crystalline flake graphite and concentrated nitric acid is 15:20-40: 80-100.

4. The multifunctional perfluorohexanone fire extinguishing agent according to claim 2, wherein the stirring reaction temperature is 20-60 ℃ and the stirring reaction time is 40-180 min.

5. The multifunctional perfluorohexanone fire extinguishing agent according to claim 2, wherein the drying temperature is 60-90 ℃ and the drying time is 10-36 h.

6. A multifunctional perfluorohexanone fire extinguishing agent according to claim 1, wherein the preparation method of chitosan-graftable poly (acrylic acid-co-methacrylamide) hydrogel comprises the steps of: dissolving a chitosan solution in an acetic acid solution, stirring and introducing nitrogen, heating to a reaction temperature, adding potassium persulfate for reaction, sequentially adding acrylic acid, acrylamide and N, N-methylene bisacrylamide, mixing, reacting, cooling to room temperature, neutralizing a reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with the ethanol, and drying to obtain the chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel.

7. The multifunctional perfluorohexanone fire extinguishing agent according to claim 6, wherein the mass ratio of the chitosan solution, the acetic acid solution, the potassium persulfate, the acrylic acid, the acrylamide, the N, N-methylene bisacrylamide is 100: 20-30: 0-1: 10-30: 15-25: 1-5.

8. The multifunctional perfluorohexanone fire extinguishing agent according to claim 6, wherein the nitrogen gas is introduced for 20-40min, the heating reaction temperature is 25-35 ℃, the time for introducing potassium persulfate for reaction is 10-20min, and the mixing reaction condition is stirring reaction at 25-35 ℃ for 3-5 h.

9. The multifunctional perfluorohexanone fire extinguishing agent according to claim 1, wherein the dispersing agent is an organophosphate compound.

Technical Field

The invention relates to the technical field of fire extinguishing agent preparation, and particularly relates to a multifunctional perfluorohexanone fire extinguishing agent and a preparation method thereof.

Background

Perfluor hexanone has a great deal of advantages such as high-efficient, clean, environmental protection as fire extinguishing agent, after it released confined space, the propagation of flame can be suppressed rapidly through physics and chemical mode to the fire extinguishing agent, and the physics gasification stage absorbs a large amount of heats, and the chemical reaction stage produces a large amount of free radicals and blocks the burning chain reaction, extinguishes flame fast, and whole fire extinguishing process puts out a fire rapidly and does not have solid, powder to remain, and the wide application is in places such as office space, market, factory building, warehouse, communication computer lab.

However, researches show that under the condition of the same fire source, the amount of toxic and corrosive gas HF generated by the clean chemical gas fire extinguishing agent is 5-10 times of that of Halon 1301 under the condition of the same fire source, HF is a toxic strong acid gas and can seriously corrode metal equipment and electronic equipment in a humid environment, irreparable damage can be caused to fire extinguishers in a fire scene after human bodies are inhaled, and the important significance is provided for better protecting the life safety of people on how to reduce the generation of the toxic gas HF generated by the clean chemical gas fire extinguishing agent in the fire extinguishing process.

Patent document CN110170141A discloses a multifunctional fire extinguishing agent and a preparation method thereof, which comprises a water-based fire extinguishing agent raw material, and also comprises the following preparation raw materials in the weight ratio of the water-based fire extinguishing agent raw material: 20-30% of perfluorohexanone, 10-15% of contact medium, 18-25% of botanical insecticide and 5-8% of dispersing agent, wherein the perfluorohexanone, the contact medium, the botanical insecticide and the dispersing agent are added according to the weight ratio on the basis of the water-based fire extinguishing agent raw material, and through the design of the specific contact medium and the matching design of the contact medium, the perfluorohexanone, the botanical insecticide and the dispersing agent, the perfluorohexanone can be rapidly cooled, and after the perfluorohexanone is mixed with the water-based fire extinguishing agent raw material, the insulation property of the mixture can be improved; in the contact medium, the inner coating layer is a mixture of platinum and palladium, so that the contact medium has good high-temperature tolerance performance, the surface area can be enlarged by mixing the catalyst and gamma-phase nano aluminum oxide, the function of preventing slag bonding is achieved, the catalyst with a spiral structure made of rare metal is attached to the surface of the inner coating layer, and the contact medium can be oxidized by the catalyst in a fire scene environment, so that the decomposition of combustion smoke and toxic gas is completed; due to the addition of the botanical insecticide, on one hand, the botanical insecticide can be well compatible with other raw materials, on the other hand, the fire extinguishing agent can achieve the functions of killing insects and expelling insects, and the requirements of green, environmental protection and safety performance are met; the dispersing agent can promote the whole mixed raw materials to form a stable dispersing system after mixing, thereby promoting the stability of the whole performance; the invention can fully mix the materials with the water-based fire extinguishing agent raw materials, so that the fire extinguishing effect of the fire extinguishing agent reaches the aim, and meanwhile, the fire extinguishing agent can play the roles of quickly cooling, removing smoke, removing toxicity and expelling insects.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention aims to provide a multifunctional perfluorohexanone fire extinguishing agent and a preparation method thereof, which can improve the insulation property of the fire extinguishing agent and solve the problem that the fire extinguishing agent has toxicity in the fire extinguishing process.

(II) technical scheme

In order to achieve the purpose, the invention adopts the following technical scheme:

the multifunctional perfluorohexanone fire extinguishing agent comprises a water-based fire extinguishing agent raw material and also comprises the following preparation raw materials in percentage by weight of the water-based fire extinguishing agent raw material: 25-35% of perfluorohexanone, 12-18% of expandable graphite, 15-20% of chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel and 8-10% of dispersing agent.

Preferably, the preparation method of the expandable graphite comprises the following steps: and (3) stirring hydrogen peroxide, flake graphite and concentrated nitric acid for reaction, and then washing and drying the obtained reaction product to obtain the expandable graphite.

Preferably, the mass ratio of the hydrogen peroxide to the crystalline flake graphite to the concentrated nitric acid is 15:20-40: 80-100.

Preferably, the stirring reaction temperature is 20-60 ℃, and the stirring reaction time is 40-180 min.

Preferably, the drying temperature is 60-90 ℃ and the drying time is 10-36 h.

Preferably, the method for preparing the chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel comprises the following steps: dissolving a chitosan solution in an acetic acid solution, stirring and introducing nitrogen, heating to a reaction temperature, adding potassium persulfate for reaction, sequentially adding acrylic acid, acrylamide and N, N-methylene bisacrylamide, mixing, reacting, cooling to room temperature, neutralizing a reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with the ethanol, and drying to obtain the chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel.

Preferably, the mass ratio of the chitosan solution to the acetic acid solution to the potassium persulfate to the acrylic acid to the acrylamide to the N, N-methylene-bis-acrylamide is 100: 20-30: 0-1: 10-30: 15-25: 1-5.

Preferably, the nitrogen is introduced for 20-40min, the heating reaction temperature is 25-35 ℃, and the time for introducing potassium persulfate for reaction is 10-20 min.

Preferably, the mixing reaction condition is that the stirring reaction is carried out for 3 to 5 hours at the temperature of between 25 and 35 ℃.

The invention also provides a preparation method of the multifunctional perfluorohexanone fire extinguishing agent, which comprises the following steps: uniformly mixing water system fire extinguishing agent raw materials, perfluorohexanone, expandable graphite, chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel and a dispersing agent to obtain the multifunctional perfluorohexanone fire extinguishing agent.

Preferably, the dispersant is an organic phosphate compound.

(III) advantageous technical effects

Compared with the prior art, the invention has the following beneficial effects:

(1) the invention provides a multifunctional perfluorohexanone fire extinguishing agent and a preparation method thereof, on the basis of a water system fire extinguishing agent raw material, the perfluorohexanone is added, so that the insulativity of the fire extinguishing agent can be improved, the aim of quickly cooling is achieved, the surface area can be enlarged by adding expandable graphite, the effect of preventing slag bonding is achieved, and in a fire scene environment, the expandable graphite can expand to absorb heat to form porous carbon so as to adsorb combustion smoke and toxic gas.

(2) Acrylic acid and methacrylamide are grafted to chitosan through a polymerization reaction to obtain chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel with excellent water absorption and higher swelling degree, the water retention and the viscosity of the water-based fire extinguishing agent are increased to a certain extent, and perfluorohexanone and expanded graphite are fixed in an interpenetrating network structure of the hydrogel, so that the compatibility among materials is improved, the hydrogel can prolong the action time of the perfluorohexanone on the surface of a fire source during fire extinguishing, the fire extinguishing effect of the fire extinguishing agent is improved, and the hydrogel can synergistically adsorb smoke and toxic gas released from the surface of the fire source, so that the fire extinguishing agent with excellent fire extinguishing performance and capable of adsorbing the smoke and the toxic gas is obtained.

Detailed Description

The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments. It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.

Example 1

A preparation method of a multifunctional perfluorohexanone fire extinguishing agent comprises the following steps:

(1) preparing expandable graphite: stirring 15g of hydrogen peroxide, 20g of flake graphite and 80g of concentrated nitric acid at 40 ℃ for 80min, washing the obtained reaction product, and drying at 60 ℃ for 12h to obtain expandable graphite;

(2) preparation of chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel: dissolving 90ml of chitosan solution in 20 acetic acid solution, stirring, introducing nitrogen for 20min, heating to the reaction temperature of 30 ℃, adding 0.5g of potassium persulfate for reaction, sequentially adding 10g of acrylic acid, 15g of acrylamide and 1g of N, N-methylene bisacrylamide, mixing and reacting at 25 ℃ for 3h, cooling to room temperature, neutralizing the reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with ethanol, and drying to obtain chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel;

(3) preparing a multifunctional perfluorohexanone fire extinguishing agent: in the embodiment, an S-6-AB-E500 water-based foam extinguishing agent is selected as a water-based extinguishing agent raw material, and 100g of the water-based extinguishing agent raw material, 25g of perfluorohexanone, 12g of expandable graphite, 15g of chitosan-grafted poly (acrylic acid-co-methacrylamide) and 8g of dispersant alkylphenol polyoxyethylene ether are uniformly mixed to obtain the multifunctional perfluorohexanone extinguishing agent.

Example 2

A preparation method of a multifunctional perfluorohexanone fire extinguishing agent comprises the following steps:

(1) preparing expandable graphite: stirring 15g of hydrogen peroxide, 25g of flake graphite and 85g of concentrated nitric acid at 30 ℃ for 120min, washing the obtained reaction product, and drying at 70 ℃ for 15h to obtain expandable graphite;

(2) preparation of chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel: dissolving 95ml of chitosan solution in 20ml of acetic acid solution, stirring and introducing nitrogen for 40min, heating to the reaction temperature of 35 ℃, adding 0.6g of potassium persulfate for reaction, then sequentially adding 15g of acrylic acid, 18g of acrylamide and 2g of N, N-methylene bisacrylamide, mixing and reacting at 30 ℃ for 4h, cooling to room temperature, neutralizing the reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with ethanol, and drying to obtain chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel;

(3) preparing a multifunctional perfluorohexanone fire extinguishing agent: in the embodiment, an S-6-AB-E500 water-based foam extinguishing agent is selected as a water-based extinguishing agent raw material, and 100g of the water-based extinguishing agent raw material, 30g of perfluorohexanone, 15g of expandable graphite, 17g of chitosan-grafted poly (acrylic acid-co-methacrylamide) and 10g of dispersant fatty amide polyoxyethylene ether are uniformly mixed to obtain the multifunctional perfluorohexanone extinguishing agent.

Example 3

A preparation method of a multifunctional perfluorohexanone fire extinguishing agent comprises the following steps:

(1) preparing expandable graphite: stirring 15g of hydrogen peroxide, 30g of flake graphite and 90g of concentrated nitric acid at 40 ℃ for 100min, washing the obtained reaction product, and drying at 80 ℃ for 18h to obtain expandable graphite;

(2) preparation of chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel: dissolving 100ml of chitosan solution in 20ml of acetic acid solution, stirring and introducing nitrogen for 40min, heating to the reaction temperature of 35 ℃, adding 0.8g of potassium persulfate for reaction, then sequentially adding 25g of acrylic acid, 20g of acrylamide and 3g of N, N-methylene bisacrylamide, mixing and reacting at 30 ℃ for 4h, cooling to room temperature, neutralizing the reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with ethanol, and drying to obtain chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel;

(3) preparing a multifunctional perfluorohexanone fire extinguishing agent: in the embodiment, an S-6-AB-E500 water-based foam extinguishing agent is selected as a water-based extinguishing agent raw material, and 100g of the water-based extinguishing agent raw material, 32g of perfluorohexanone, 17g of expandable graphite, 19g of chitosan-grafted poly (acrylic acid-co-methacrylamide) and 9g of dispersant fatty amide polyoxyethylene ether are uniformly mixed to obtain the multifunctional perfluorohexanone extinguishing agent.

Example 4

A preparation method of a multifunctional perfluorohexanone fire extinguishing agent comprises the following steps:

(1) preparing expandable graphite: stirring 15g of hydrogen peroxide, 38g of flake graphite and 100g of concentrated nitric acid at 55 ℃ for 150min, washing the obtained reaction product, and drying at 75 ℃ for 28h to obtain expandable graphite;

(2) preparation of chitosan-grafted poly (acrylic acid-co-methacrylamide) hydrogel: dissolving 100ml of chitosan solution in 20ml of acetic acid solution, stirring and introducing nitrogen for 40min, heating to the reaction temperature of 35 ℃, adding 1g of potassium persulfate for reaction, then sequentially adding 30g of acrylic acid, 25g of acrylamide and 5g of N, N-methylene bisacrylamide, mixing and reacting at 30 ℃ for 4h, cooling to room temperature, neutralizing the reactant until the pH value is 7, adding excessive ethanol to separate out a product of graft polymerization, repeatedly washing with ethanol, and drying to obtain chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel;

(3) preparing a multifunctional perfluorohexanone fire extinguishing agent: in the embodiment, an S-6-AB-E500 water-based foam extinguishing agent is selected as a water-based extinguishing agent raw material, and 100g of the water-based extinguishing agent raw material, 35g of perfluorohexanone, 18g of expandable graphite, 20g of chitosan-grafted poly (acrylic acid-co-methacrylamide) and 10g of dispersant alkylphenol polyoxyethylene ether are uniformly mixed to obtain the multifunctional perfluorohexanone extinguishing agent.

Comparative example 1

As a comparative example, an S-6-AB-E500 aqueous foam extinguishing agent was used as it is.

Comparative example 2

A preparation method of a multifunctional perfluorohexanone fire extinguishing agent comprises the following steps:

(1) preparing expandable graphite: stirring 15g of hydrogen peroxide, 38g of flake graphite and 100g of concentrated nitric acid at 55 ℃ for 150min, washing the obtained reaction product, and drying at 75 ℃ for 28h to obtain expandable graphite;

(2) preparing a multifunctional perfluorohexanone fire extinguishing agent: in the embodiment, an S-6-AB-E500 water-based foam extinguishing agent is selected as a water-based extinguishing agent raw material, and 100g of the water-based extinguishing agent raw material, 25g of perfluorohexanone, 12g of expandable graphite and 10g of dispersant alkylphenol polyoxyethylene ether are uniformly mixed to obtain the multifunctional perfluorohexanone extinguishing agent.

The multifunctional perfluorohexanone fire extinguishing agent obtained in the examples 1-4 and the comparative examples 1-2 is subjected to performance detection, and the specific detection method is as follows:

fire extinguishing performance: and testing the fire extinguishing performance of the test piece according to GB 15308.

	Time of fire extinguishing/s	Burn resistance time/min	State of smoke
				Example 1	52s	16.3	Is free of
Example 2	47s	23.9	Is free of
				Example 3	36s	26.2	Is free of
Example 4	35s	27.4	Is free of
				Comparative example 1	78s	10.5	Is provided with
Comparative example 2	62s	12.2	Is provided with

From the above table of examples 1-4, it can be seen that with the increase in the composition of perfluorohexanone, expandable graphite and chitosan-grafted poly (acrylic acid-co-methacrylamide), the fire extinguishing properties, fire resistance of the fire extinguishing agent are increased, and smoke is greatly reduced. In comparison with example 1, it can be seen that the fire extinguishing performance is greatly lowered and there is smoke in comparative example 1. Compared with the example 1, the fire extinguishing agent without the chitosan grafted poly (acrylic acid-co-methacrylamide) has the overall performance reduced, which shows that the chitosan grafted poly (acrylic acid-co-methacrylamide) hydrogel plays an indispensable role in the fire extinguishing agent, not only enhances the water retention of the fire extinguishing agent, but also enhances the effects of perfluorohexanone and expandable graphite on the surface of a fire source, so as to carry out synergistic fire extinguishing and obtain the fire extinguishing agent with excellent fire extinguishing performance and capable of adsorbing smoke and toxic gas.

Finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.