Fire extinguishing agent

Abstract

The invention discloses a fire extinguishing agent which comprises 5-10 parts of modified MOF and 10-20 parts of modified polyethylene glycol hydrogel. The fire extinguishing agent has the beneficial effects that the prepared fire extinguishing agent can effectively cover, cool and cool a target area on the surface of a vertical combustion body, the water retention performance of the fire extinguishing agent is stable in a high-temperature or dry environment, the gel layer does not shrink or pulverize, and the lasting fire extinguishing effect is kept.

Description

Technical Field

[0001] The invention belongs to the technical field of fire extinguishing agents, and in particular relates to a fire extinguishing agent. Background Art

[0002] Water is the most commonly used fire extinguishing agent, with the advantages of strong heat absorption capacity, easy access, and low cost. However, ordinary water has good fluidity and is easy to volatilize at high temperatures, which makes it difficult to stay on combustibles and cannot fully exert its fire extinguishing performance. In order to improve these shortcomings, people add surfactants, inorganic salts and other additives to water, or treat water by ultrafine, atomization and other treatments to improve the fire extinguishing performance of water. Such fire extinguishing agents are generally referred to as water-based fire extinguishing agents. Hydrogel fire extinguishing agent is also a kind of water-based fire extinguishing agent. Its main component is hydrogel material, which is a high-water gel-like substance with a three-dimensional network structure formed by adding natural substances or chemically synthesized substances to water and chemically or physically cross-linking. This type of fire extinguishing agent has good adhesion, water retention and oxygen isolation, and can form a moisturizing layer and a heat-insulating and oxygen-insulating layer on the surface of the fire source to effectively curb the spread of the fire. As a new type of fire extinguishing agent, hydrogel fire extinguishing agent has outstanding advantages. Its application in different scenarios such as industrial fires, building fires and forest fires has been reported in a large number of literatures, fully demonstrating its wide applicability.

[0003] However, the hydrogel fire extinguishing agent has a low adhesion thickness on the surface of vertical walls or complex structures, which makes it impossible to effectively cover, cool and reduce the temperature of the target area, thus affecting the fire extinguishing effect. Although the hydrogel fire extinguishing agent can quickly absorb a large amount of water and expand to form a gel layer in the early stage, its water retention performance may gradually decrease over time, especially in high temperature or dry environment, causing the gel layer to shrink or even powderize, thus affecting its long-lasting fire extinguishing effect. In order to solve the existing problems, we propose a fire extinguishing agent. Summary of the invention

[0004] The object of the present invention is to provide a fire extinguishing agent to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A fire extinguishing agent comprises 5-10 parts of modified MOF and 10-20 parts of modified polyethylene glycol hydrogel.

[0007] Preferably, the preparation steps of the modified polyethylene glycol hydrogel include:

[0008] S1: Ethylene glycol is stirred in dimethyl sulfoxide until the mixture is uniform, sodium is added, and process condition 1 is set. After the reaction is completed, intermediate 1 is obtained;

[0009] S2: octamethylcyclotetrasiloxane and intermediate 1 are mixed in a certain weight ratio, process conditions are set, and inert gas protection is applied, and finally an appropriate amount of methacrylic acid is added to obtain intermediate 2;

[0010] S3: Dissolve the intermediate 2, PEG and butyl methacrylate in ethyl acetate, add BPO, and react at an appropriate temperature. After the reaction is completed, purify to obtain modified PEG;

[0011] S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution;

[0012] S5: taking appropriate amounts of methyl cellulose aqueous solution and modified polyethylene glycol aqueous solution, mixing them evenly and swelling them to obtain intermediate 3;

[0013] S6: Add an appropriate amount of sodium chloride NaCl aqueous solution to the intermediate 3, and obtain the modified polyethylene glycol hydrogel after defoaming.

[0014] Preferably,

[0015] The mass fractions of methylcellulose and modified polyethylene glycol PEG are 1-3% and 3-6% respectively; the mass fraction of sodium chloride is 3-7%;

[0016] The mass ratios of the methylcellulose aqueous solution, the modified polyethylene glycol powder aqueous solution and the sodium chloride aqueous solution are 20-30 parts: 40-60 parts and 30-50 parts.

[0017] Preferably,

[0018] In step S1, the mass ratio of ethylene glycol, dimethyl sulfoxide, and sodium is 10-20 parts; 10-30 parts: 1-5 parts;

[0019] In step S2, the mass ratio of octamethylcyclotetrasiloxane to intermediate 1 is 10-20 parts and 5-10 parts;

[0020] In step S3, the mass ratio of intermediate 2, PEG, butyl methacrylate, ethyl acetate and BPO is 1-3 parts: 10-20 parts; 2-5 parts; 20-50 parts, 2-4 parts.

[0021] Preferably,

[0022] The process conditions of step S1 are a temperature of 20-50°C and a time of 1-5h;

[0023] The process conditions of step S2 are temperature 30-80°C and reaction time 1-5h;

[0024] The process conditions of step S3 are temperature 50-80°C and time 0.5-3h;

[0025] The mixing process conditions in step S5 are a temperature of 50-70° C., stirring, a stirring rate of 300-800 r / min, a time of 2-3 h, and standing at room temperature for more than 8 hours;

[0026] In step S6, the temperature is 50-60° C., and stirring is performed at a stirring rate of 100-300 r / min for 2-3 hours, and the mixture is allowed to stand at room temperature for more than 12 hours.

[0027] Preferably, the preparation steps of the modified MOF include:

[0028] T1: Add appropriate amount of ZrCl4 and terephthalic acid into DMF, add appropriate amount of glacial acetic acid, mix well, and prepare intermediate a;

[0029] T2: Transfer intermediate a to a reactor, perform crystallization treatment, purify and dry in a vacuum or oven to obtain intermediate b;

[0030] T3: Add a certain amount of 2-aminoterephthalic acid and intermediate b into DMF to obtain intermediate c; continue to add an appropriate amount of AgNO3, stir to obtain intermediate e, crystallize for a certain period of time and purify to obtain modified MOF.

[0031] Preferably, the mass ratio of ZrCl4, terephthalic acid, DMF, and glacial acetic acid is 10-20 parts: 20-30 parts: 20-50 parts: 1-3 parts; the mass ratio of 2-aminoterephthalic acid, intermediate b, DMF, and AgNO3 is 10-20 parts: 20-30 parts: 20-50 parts: 1-3 parts.

[0032] Preferably, the crystallization treatment temperature of step T2 is 80-120° C. and the time is 1-3 h; the crystallization temperature of step T3 is 80-120° C. and the time is 0.5-2 h.

[0033] Compared with the prior art, the beneficial effects of the present invention are: the fire extinguishing agent prepared by the present invention can effectively cover, cool and reduce the temperature of the target area on the surface of the vertical combustion body, and its water retention performance is stable in high temperature or dry environment, the gel layer will not shrink or powder, and maintain a lasting fire extinguishing effect. DETAILED DESCRIPTION

[0034] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions 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. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0035] Embodiment 1:

[0036] Step 1: Preparation of modified polyethylene glycol hydrogel

[0037] S1: 10 parts of ethylene glycol are stirred in 10 parts of dimethyl sulfoxide until the mixture is uniform, and 1 part of sodium is added. The process conditions are set at a temperature of 20°C and a reaction time of 1 hour. After the reaction is completed, intermediate 1 is obtained.

[0038] S2: 10 parts of octamethylcyclotetrasiloxane and 5 parts of intermediate 1 were mixed in a certain weight ratio, the process conditions were set at a temperature of 30°C, the reaction time was 1 hour, and inert gas protection was applied, and finally an appropriate amount of methacrylic acid was added to obtain intermediate 2;

[0039] S3: Dissolve 1 part of intermediate 2, 10 parts of PEG and 2 parts of butyl methacrylate in 20 parts of ethyl acetate, add 2 parts of BPO, and react at an appropriate temperature. The process conditions are 50°C and 0.5h. After the reaction is completed, purify to obtain modified PEG;

[0040] S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution;

[0041] S5: 20 parts by mass of a 1% aqueous solution of methyl cellulose and 40 parts by mass of a 3-6% aqueous solution of modified polyethylene glycol are mixed evenly and swelled. The mixing process conditions are a temperature of 50° C. and stirring at a stirring rate of 300 r / min for 2 h. The mixture is allowed to stand at room temperature for more than 8 hours to obtain an intermediate 3.

[0042] S6: Add 30 parts of 3% sodium chloride NaCl aqueous solution to the intermediate 3 at 50°C, stir at a rate of 100 r / min for 2 hours, and let stand at room temperature for 13 hours to obtain a modified polyethylene glycol hydrogel.

[0043] Step 2: Preparation of modified MOF:

[0044] T1: 10 parts of ZrCl4 and 20 parts of terephthalic acid are added to 20 parts of DMF, and 1 part of glacial acetic acid is added, and mixed evenly to prepare intermediate a;

[0045] T2: Transfer intermediate a to a reactor, perform crystallization treatment at 80°C for 1 hour, purify and dry in a vacuum or oven to obtain intermediate b;

[0046] T3: 10 parts of 2-aminoterephthalic acid and 20 parts of intermediate b were added to 20 parts of DMF to obtain intermediate c; 1 part of AgNO3 was added and stirred to obtain intermediate e, which was crystallized at 80°C for 0.5h and purified to obtain modified MOF.

[0047] 5 parts of modified MOF and 10 parts of modified polyethylene glycol hydrogel were mixed.

[0048] Embodiment 2:

[0049] Step 1: Preparation of modified polyethylene glycol hydrogel

[0050] S1: 20 parts of ethylene glycol were stirred in 30 parts of dimethyl sulfoxide until the mixture was uniform, and 5 parts of sodium were added. The process conditions were set at a temperature of 50°C and a reaction time of 5 hours. After the reaction was completed, intermediate 1 was obtained.

[0051] S2: 20 parts of octamethylcyclotetrasiloxane and 10 parts of intermediate 1 were mixed in a certain weight ratio, the process conditions were set to a temperature of 80°C, the reaction time was 5 hours, and inert gas protection was applied, and finally an appropriate amount of methacrylic acid was added to obtain intermediate 2;

[0052] S3: 3 parts of intermediate 2, 20 parts of PEG and 5 parts of butyl methacrylate were dissolved in 50 parts of ethyl acetate, and 4 parts of BPO were added to react at an appropriate temperature. The process conditions were 80°C and 3 hours. After the reaction was completed, the modified PEG was purified;

[0053] S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution;

[0054] S5: 30 parts by mass of a 1-3% aqueous solution of methyl cellulose and 60 parts by mass of a 6% aqueous solution of modified polyethylene glycol are mixed evenly and swelled. The mixing process conditions are a temperature of 70° C., stirring at a stirring rate of 800 r / min for 3 hours, and standing at room temperature for more than 8 hours to obtain an intermediate 3;

[0055] S6: Add 50 parts of 7% sodium chloride NaCl aqueous solution to the intermediate 3 at 60°C, stir at a rate of 300 r / min for 3 hours, and let stand at room temperature for 15 hours to obtain a modified polyethylene glycol hydrogel.

[0056] Step 2: Preparation of modified MOF:

[0057] T1: 20 parts of ZrCl4 and 30 parts of terephthalic acid were added to 50 parts of DMF, and 3 parts of glacial acetic acid were added, and mixed well to prepare intermediate a;

[0058] T2: Transfer intermediate a to a reactor, perform crystallization treatment at 120°C for 3 hours, purify and dry in a vacuum or oven to obtain intermediate b;

[0059] T3: Add 20 parts of 2-aminoterephthalic acid and 30 parts of intermediate b into 50 parts of DMF to obtain intermediate c; continue to add 3 parts of AgNO3, stir to obtain intermediate e, crystallize at 120°C for 2h, and obtain modified MOF after purification.

[0060] 10 parts of modified MOF and 20 parts of modified polyethylene glycol hydrogel were mixed.

[0061] Embodiment 3:

[0062] Step 1: Preparation of modified PEG hydrogel

[0063] S1: 15 parts of ethylene glycol were stirred in 16 parts of dimethyl sulfoxide until the mixture was uniform, and 3 parts of sodium were added. The process conditions were set at a temperature of 30°C and a reaction time of 3 hours. After the reaction was completed, intermediate 1 was obtained.

[0064] S2: 15 parts of octamethylcyclotetrasiloxane and 8 parts of intermediate 1 were mixed in a certain weight ratio, the process conditions were set to a temperature of 50°C, the reaction time was 3 hours, and inert gas protection was applied, and finally an appropriate amount of methacrylic acid was added to obtain intermediate 2;

[0065] S3: Dissolve 2 parts of intermediate 2, 15 parts of PEG and 4 parts of butyl methacrylate in 40 parts of ethyl acetate, add 3 parts of BPO, and react at an appropriate temperature. The process conditions are temperature 60°C and time 2 hours. After the reaction is completed, purify and obtain modified PEG;

[0066] S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution;

[0067] S5: 25 parts by mass of a 2% aqueous solution of methyl cellulose and 50 parts by mass of a 5% aqueous solution of modified polyethylene glycol were mixed evenly and swollen. The mixing process conditions were a temperature of 60° C. and stirring at a stirring rate of 500 r / min for 2.3 h. The mixture was allowed to stand at room temperature for 9 hours to obtain an intermediate 3.

[0068] S6: Add 35 parts of 6% sodium chloride NaCl aqueous solution to the intermediate 3 at 55°C, stir at a rate of 200 r / min for 2.5 hours, and let stand at room temperature for more than 20 hours to obtain a modified polyethylene glycol hydrogel.

[0069] Step 2: Preparation of modified MOF:

[0070] T1: 15 parts of ZrCl4 and 25 parts of terephthalic acid were added to 25 parts of DMF, and 2.5 parts of glacial acetic acid were added, and mixed well to prepare intermediate a;

[0071] T2: Transfer intermediate a to a reactor, perform crystallization treatment at 100°C for 1.3 hours, purify and dry in a vacuum or oven to obtain intermediate b;

[0072] T3: 18 parts of 2-aminoterephthalic acid and 23 parts of intermediate b were added to 29 parts of DMF to obtain intermediate c; 1.3 parts of AgNO3 were added and stirred to obtain intermediate e, which was crystallized at 100°C for 1.5h and purified to obtain modified MOF.

[0073] 8 parts of modified MOF and 15 parts of modified polyethylene glycol hydrogel were mixed.

[0074] Comparative Example 1:

[0075] S1: 15 parts of ethylene glycol were stirred in 16 parts of dimethyl sulfoxide until the mixture was uniform, and 3 parts of sodium were added. The process conditions were set at a temperature of 30°C and a reaction time of 3 hours. After the reaction was completed, intermediate 1 was obtained.

[0076] S2: 15 parts of octamethylcyclotetrasiloxane and 8 parts of intermediate 1 were mixed in a certain weight ratio, the process conditions were set to a temperature of 50°C, the reaction time was 3 hours, and inert gas protection was applied, and finally an appropriate amount of methacrylic acid was added to obtain intermediate 2;

[0077] S3: Dissolve 2 parts of intermediate 2, 15 parts of PEG and 4 parts of butyl methacrylate in 40 parts of ethyl acetate, add 3 parts of BPO, and react at an appropriate temperature. The process conditions are temperature 60°C and time 2 hours. After the reaction is completed, purify and obtain modified PEG;

[0078] S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution;

[0079] S5: 25 parts by mass of a 2% aqueous solution of methyl cellulose and 50 parts by mass of a 5% aqueous solution of modified polyethylene glycol were mixed evenly and swollen. The mixing process conditions were a temperature of 60° C. and stirring at a stirring rate of 500 r / min for 2.3 h. The mixture was allowed to stand at room temperature for 9 hours to obtain an intermediate 3.

[0080] S6: Add 35 parts of 6% sodium chloride NaCl aqueous solution to the intermediate 3 at 55°C, stir at a rate of 200 r / min for 2.5 hours, and let stand at room temperature for more than 20 hours to obtain a modified polyethylene glycol hydrogel.

[0081] Comparative Example 2:

[0082] T1: 15 parts of ZrCl4 and 25 parts of terephthalic acid were added to 25 parts of DMF, and 2.5 parts of glacial acetic acid were added, and mixed well to prepare intermediate a;

[0083] T2: Transfer intermediate a to a reactor, perform crystallization treatment at 100°C for 1.3 hours, purify and dry in a vacuum or oven to obtain intermediate b;

[0084] T3: 18 parts of 2-aminoterephthalic acid and 23 parts of intermediate b were added to 29 parts of DMF to obtain intermediate c; 1.3 parts of AgNO3 were added and stirred to obtain intermediate e, which was crystallized at 100°C for 1.5h and purified to obtain modified MOF.

[0085] Comparative Example 3: Water

[0086] The products prepared in Example 1-3 and Comparative Example 1-2 were diluted with water to a 2wt% aqueous solution and emulsified at an emulsifier speed of 500-1000r / min for 20-30min. Then, a wood pile dry burning experiment was conducted. One side of the wood pile was vertically arranged side by side. When extinguishing the fire, spray was applied toward the vertical surface. The specific test results are as follows:

[0087] Table 1 Test results

[0088]

[0089] From the results in Table 1, we can see that

[0090] In Examples 1-3, the fire control time was between 4 and 6 seconds, and the fire extinguishing time was between 35 and 40 seconds, and no re-ignition occurred. 2.8 to 3.1 L of fire extinguishing agent was used during the fire extinguishing process, and no shrinkage or powdering occurred after the fire was extinguished.

[0091] Compared with Comparative Example 3, Examples 1-3 failed to control the fire when using water, indicating that the fire extinguishing agent prepared by the present invention has better performance than water.

[0092] Compared with Example 1, when using a larger amount of Example 1, the fire control time was extended by about 3-5 times, the fire extinguishing time was extended by more than double, and even re-ignition occurred after 150s, and the gel layer shrank after the fire was extinguished.

[0093] Compared with Example 3, when using a larger amount of Example 1, the fire control time was extended by about 5-7 times, the fire extinguishing time was extended by more than double, and even re-ignition occurred after 90s. Moreover, the gel layer shrank after the fire was extinguished, and powder appeared.

[0094] Although embodiments of the present invention have been shown and described (see the above detailed description for details), it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A fire extinguishing agent, characterized in that: The invention comprises 5-10 parts of modified MOF and 10-20 parts of modified polyethylene glycol hydrogel.

2. A fire extinguishing agent according to claim 1, characterized in that: The preparation steps of the modified polyethylene glycol hydrogel include: S1: Ethylene glycol is stirred in dimethyl sulfoxide until the mixture is uniform, sodium is added, and process condition 1 is set. After the reaction is completed, intermediate 1 is obtained; S2: octamethylcyclotetrasiloxane and intermediate 1 are mixed in a certain weight ratio, process conditions are set, and inert gas protection is applied, and finally an appropriate amount of methacrylic acid is added to obtain intermediate 2; S3: Dissolve the intermediate 2, PEG and butyl methacrylate in ethyl acetate, add BPO, and react at an appropriate temperature. After the reaction is completed, purify to obtain modified PEG; S4: taking an appropriate amount of the modified polyethylene glycol prepared in S3 to prepare a modified polyethylene glycol aqueous solution; S5: taking appropriate amounts of methyl cellulose aqueous solution and modified polyethylene glycol aqueous solution, mixing them evenly and swelling them to obtain intermediate 3; S6: Add an appropriate amount of sodium chloride NaCl aqueous solution to the intermediate 3, and obtain the modified polyethylene glycol hydrogel after defoaming.

3. A fire extinguishing agent according to claim 2, characterized in that: The mass fractions of the methyl cellulose and the modified polyethylene glycol PEG are 1-3% and 3-6% respectively; the mass fraction of the sodium chloride is 3-7%; The mass ratios of the methyl cellulose aqueous solution, the modified polyethylene glycol powder aqueous solution and the sodium chloride aqueous solution are 20-30 parts, 40-60 parts and 30-50 parts.

4. A fire extinguishing agent according to claim 2, characterized in that: In step S1, the mass ratio of ethylene glycol, dimethyl sulfoxide and sodium is 10-20 parts; 10-30 portions: 1-5 portions; In step S2, the mass ratio of octamethylcyclotetrasiloxane to intermediate 1 is 10-20 parts and 5-10 parts; In step S3, the mass ratio of intermediate 2, PEG, butyl methacrylate, ethyl acetate and BPO is 1-3 parts: 10-20 parts; 2-5 parts; 20-50 parts, 2-4 parts.

5. A fire extinguishing agent according to claim 2, characterized in that: The process conditions of step S1 are a temperature of 20-50°C and a time of 1-5h; The process conditions of step S2 are a temperature of 30-80°C and a reaction time of 1-5h; The process conditions of step S3 are a temperature of 50-80°C and a time of 0.5-3h; The mixing process conditions in step S5 are a temperature of 50-70° C., stirring, a stirring rate of 300-800 r / min, a time of 2-3 h, and standing at room temperature for more than 8 hours; In step S6, the temperature is 50-60° C., and stirring is performed at a stirring rate of 100-300 r / min for 2-3 hours, and the mixture is allowed to stand at room temperature for more than 12 hours.

6. A fire extinguishing agent according to claim 1, characterized in that: The preparation steps of the modified MOF include: T1: Add appropriate amount of ZrCl4 and terephthalic acid into DMF, add appropriate amount of glacial acetic acid, mix well, and prepare intermediate a; T2: Transfer intermediate a to a reactor, perform crystallization treatment, purify and dry in a vacuum or oven to obtain intermediate b; T3: Add a certain amount of 2-aminoterephthalic acid and intermediate b into DMF to obtain intermediate c; continue to add an appropriate amount of AgNO3, stir to obtain intermediate e, crystallize for a certain period of time and purify to obtain modified MOF.

7. A fire extinguishing agent according to claim 6, characterized in that: The mass ratio of ZrCl4, terephthalic acid, DMF, and glacial acetic acid is 10-20 parts: 20-30 parts: 20-50 parts: 1-3 parts; the mass ratio of 2-aminoterephthalic acid, intermediate b, DMF, and AgNO3 is 10-20 parts: 20-30 parts: 20-50 parts: 1-3 parts.

8. A fire extinguishing agent according to claim 6, characterized in that: The crystallization treatment temperature of step T2 is 80-120° C. and the time is 1-3 hours; the crystallization temperature of step T3 is 80-120° C. and the time is 0.5-2 hours.

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