Preparation method of fire extinguishing agent special for textiles

Abstract

The invention discloses a preparation method of a fire extinguishing agent special for textiles, which comprises the following steps: S1, adding glucolactone GDL and calcium carbonate into water, and stirring and dissolving for 1 hour at a constant temperature of 45 DEG C to obtain a first mixed solution; s2, adding 20% of water into the first mixed solution, then adding lignin and hydroxyethyl cellulose, and stirring and dissolving for 2 hours at the constant temperature of 45 DEG C to obtain a second mixed solution; s3, adding an organic phosphorus-containing flame retardant, a short-chain cationic fluorocarbon surfactant, a preservative and water into the second mixed solution; and S4, finally stirring for 3 hours, and adjusting the pH value to be neutral to obtain the fire extinguishing agent. The self-made and synthesized organic phosphorus-containing flame retardant can inhibit generation of a combustible substance intermediate, namely levoglucose, in the cotton fiber cracking process at a high temperature, and meanwhile, the prepared fire extinguishing agent can be spread to form a thin gel film after being sprayed on the surface of a comburent, so that air can be effectively isolated, and combustion can be inhibited by cooling; after fire extinguishing, the gel film is easy to clean, and reuse of the textile is not affected.

Description

Technical Field

[0001] The invention relates to the technical field of fire fighting, and in particular to a method for preparing a special fire extinguishing agent for textiles. Background Art

[0002] At present, cotton-containing textiles are easy to burn. Once burning, it is easy for cotton-containing textiles to get out of control and form charcoal ash after complete combustion. Therefore, in textile production workshops and warehouses, once a fire occurs, the fire is very easy to get out of control and difficult to extinguish. Traditional fire-fighting technology may not be able to effectively deal with textile fires, and often has problems such as slow extinguishing speed and incomplete fire extinguishing, or after the fire is extinguished, the textiles are contaminated and scrapped or difficult to clean.

[0003] Therefore, how to efficiently and quickly extinguish fires of cotton-containing textiles, and impart flame retardant properties to cotton-containing textiles, so as to suppress, control and extinguish fires in the early stages of fires, is an urgent problem to be solved by those skilled in the art. Summary of the invention

[0004] One object of the present invention is to provide a method for preparing a special fire extinguishing agent for textiles. The present invention can inhibit the formation of levorotatory glucose, a combustible intermediate, during the cracking process of cotton fibers at high temperatures through a self-made synthetic organic phosphorus-containing flame retardant. At the same time, the prepared fire extinguishing agent can be spread on the surface of the burning object to form a thin layer of gel film, which can effectively isolate the air, cool down and inhibit combustion. After the fire is extinguished, the gel film is easy to clean and does not affect the reuse of the textile.

[0005] A method for preparing a special fire extinguishing agent for textiles according to an embodiment of the present invention comprises the following steps:

[0006] S1, adding gluconolactone GDL and calcium carbonate into water, wherein the addition percentages of water, gluconolactone and calcium carbonate are 10%, 2% and 1% respectively, and stirring and dissolving at a constant temperature of 45° C. for 1 hour to obtain a first mixed solution;

[0007] S2, adding 20% ​​water to the first mixed solution, and then adding lignin and hydroxyethyl cellulose, wherein the addition percentage of lignin and hydroxyethyl cellulose is 3%, and then stirring and dissolving at a constant temperature of 45° C. for 2 hours to obtain a second mixed solution;

[0008] S3, adding an organic phosphorus-containing flame retardant, a short-chain cationic fluorocarbon surfactant, a preservative and water to the second mixed liquid, wherein the addition percentages of the organic phosphorus-containing flame retardant, the short-chain cationic fluorocarbon surfactant and the preservative are 10%, 2% and 1% respectively, and the remaining 48% is water;

[0009] S4. Finally, stir for 3 hours and test the pH value. Use a pH adjuster to adjust the pH to neutral to obtain a special fire extinguishing agent.

[0010] Furthermore, the preparation method of the organic phosphorus-containing flame retardant in S3 is as follows:

[0011] S311. First, add bis(2-hydroxyethyl)amino(trihydroxymethyl)methane and phosphoric acid into a three-necked flask equipped with a mechanical stirrer and a thermometer;

[0012] S312, then heated at 135°C for 2h;

[0013] S313, then under mechanical stirring at 120° C., urea was added to the beaker and stirred for 2.5 h to obtain a milky yellow fluid;

[0014] S314, purifying by washing with ethanol precipitation, and finally drying the purified product in an oven at 80° C. to obtain an organic phosphorus-containing flame retardant.

[0015] Furthermore, the preparation method of the short-chain cationic fluorocarbon surfactant in S3 is as follows:

[0016] S321, firstly, adding hexylsulfonyl fluoride to toluene, and stirring magnetically at room temperature, and adding 3-dimethylpropylenediamine dropwise during stirring;

[0017] S322, then continue to react under magnetic stirring overnight at room temperature and filter, wash the filter cake with toluene, water and ethanol in turn and dry to obtain a light yellow solid;

[0018] S323, then adding potassium iodide to butanone, adding 1-chloropinacolone after magnetic stirring for 5 minutes, stirring the reaction for 3 hours and filtering;

[0019] S324, washing the filter cake with ethanol and then using 50°C rotary evaporation until there is no fraction, then adding ethanol and the light yellow solid obtained in the reaction of S32, and reflux reaction for 6h;

[0020] S325. Finally, cool to room temperature and evaporate until there is no fraction, to obtain a red viscous solid short-chain cationic fluorocarbon surfactant.

[0021] Furthermore, a dust-free mechanical stirring device is used in all stirring steps from S1 to S4.

[0022] Furthermore, the stirring speed in all the stirring steps in S1-S4 is between 100 and 300 rpm.

[0023] Furthermore, the weight ratio of the organic phosphorus-containing flame retardant to the short-chain cationic fluorocarbon surfactant in S3 is controlled to be 5:1 to 10:1.

[0024] Furthermore, the pH value of the fire extinguishing agent is adjusted within a range of 6.5 to 7.5.

[0025] Furthermore, a large amount of yellow solid is precipitated after N,N-dimethyl-1,3-propylenediamine is added dropwise to S321, and mechanical stirring is adopted for stirring.

[0026] Furthermore, the pH value test in S4 is performed using pH test paper, and the specific steps are:

[0027] S41. Place the fire extinguishing agent to be tested into a container;

[0028] S42. Place the pH test paper in the fire extinguisher and take it out after 2 to 3 seconds;

[0029] S43. Wait for the pH test paper to change color and then compare it with the color comparison card to determine the pH.

[0030] The beneficial effects of the present invention are:

[0031] The fire extinguishing agent specially prepared for cotton-containing textiles is prepared by a self-made synthetic organic phosphorus-containing flame retardant which decomposes at high temperature to generate phosphoric acid, which then becomes metaphosphoric acid, and then condenses into polymetaphosphoric acid, thereby phosphorylating and dehydrating cotton fibers and converting them into carbon, thereby inhibiting the generation of levorotatory glucose, an intermediate of a combustible substance, during the cracking process of the cotton fibers. At the same time, the prepared fire extinguishing agent is sprayed on the surface of the burning object through equipment, and can spread to form a thin layer of gel film, which can effectively isolate the air, cool down and inhibit combustion. At the same time, after the fire extinguishing is completed, the gel film is easy to clean and does not affect the reuse of the textiles. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0033] Figure 1 This is an infrared image of a short-chain fluorocarbon surfactant in a method for preparing a special fire extinguishing agent for textiles proposed by the present invention;

[0034] Figure 2 This is a flame retardant reaction diagram of an organic phosphorus-containing flame retardant in a method for preparing a special fire extinguishing agent for textiles proposed by the present invention;

[0035] Figure 3 This is an experimental comparison diagram of a method for preparing a special fire extinguishing agent for textiles proposed by the present invention. It can be seen that the control cotton-containing textile is very easy to burn and finally burns into charcoal fire, while the cotton-containing textile sprayed with the fire extinguishing agent of the present application hardly burns at the moment of fire.

[0036] Figure 4 This is a picture of cotton textiles after being washed and dried after being extinguished by the fire extinguishing agent of the present application.

[0037] Figure 5This is an experimental thermocouple diagram of a method for preparing a special fire extinguishing agent for textiles proposed by the present invention. DETAILED DESCRIPTION

[0038] The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic diagrams, which only illustrate the basic structure of the present invention in a schematic manner, and therefore only show the components related to the present invention.

[0039] A method for preparing a special fire extinguishing agent for textiles comprises the following steps:

[0040] S1, adding gluconolactone GDL and calcium carbonate into water, wherein the addition percentages of water, gluconolactone and calcium carbonate are 10%, 2% and 1% respectively, and stirring and dissolving at a constant temperature of 45° C. for 1 hour to obtain a first mixed solution;

[0041] Among them, gluconolactone (GDL) is a food additive and acidity regulator. After dissolving in water, it reacts with water to produce gluconic acid; this is a slow hydrolysis reaction, the reaction is as follows:

[0042]

[0043] Gluconolactone (GDL formula: C6H10O6) reacts with water to produce gluconic acid (C6H11O7);

[0044] Calcium carbonate (CaCO3) does not undergo significant chemical reactions in water because it is a relatively insoluble salt. However, in an acidic environment, calcium carbonate can gradually dissolve to produce carbonate and calcium ions. The reaction process is as follows:

[0045]

[0046] In the above reaction, gluconolactone is converted into gluconic acid in water, which increases the acidity of the mixture. Therefore, calcium carbonate will gradually dissolve in this environment. The calcium ions produced by this reaction help to change the properties of the fire extinguishing agent, such as improving its adhesion to textiles and improving the fire extinguishing effect of the fire extinguishing agent.

[0047] The combination of gluconolactone and calcium carbonate will play a role in adjusting the pH value of the fire extinguishing agent, enhancing stability and performance, and improving its binding properties with textiles;

[0048] S2, adding 20% ​​water to the first mixed solution, and then adding lignin and hydroxyethyl cellulose, wherein the addition percentage of lignin and hydroxyethyl cellulose is 3%, and then stirring and dissolving at a constant temperature of 45° C. for 2 hours to obtain a second mixed solution;

[0049] Among them, lignin is a natural organic polymer with good dispersibility and stability. In the second mixed liquid, the combination of lignin, gluconic acid and calcium carbonate forms a stable complex, which helps to improve the adhesion of the fire extinguishing agent on the textile, improve the durability and flame retardant performance of the fire extinguishing agent under flames, and in addition, the addition of lignin can also improve the anti-oxidation and corrosion resistance of the fire extinguishing agent.

[0050] Secondly, hydroxyethyl cellulose is a water-soluble polymer with thickening, gelling, stabilizing and adhesive properties. In the second mixed liquid, the addition of hydroxyethyl cellulose helps to adjust the viscosity and fluidity of the fire extinguishing agent and ensure the uniform coating of the fire extinguishing agent on the textiles. In addition, hydroxyethyl cellulose can also enhance the adhesion of the fire extinguishing agent on the textiles and improve its water washability.

[0051] S3, adding an organic phosphorus-containing flame retardant, a short-chain cationic fluorocarbon surfactant, a preservative and water to the second mixed liquid, wherein the addition percentages of the organic phosphorus-containing flame retardant, the short-chain cationic fluorocarbon surfactant and the preservative are 10%, 2% and 1% respectively, and the remaining 48% is water;

[0052] Wherein, the weight ratio of the organic phosphorus-containing flame retardant to the short-chain cationic fluorocarbon surfactant is controlled to be 5:1 to 10:1.

[0053] Embodiment 1

[0054] refer to Figure 2 , the preparation method of the organic phosphorus-containing flame retardant is as follows:

[0055] S311. First, add bis(2-hydroxyethyl)amino(trihydroxymethyl)methane and phosphoric acid into a beaker equipped with a mechanical stirrer and a thermometer;

[0056] S312, then heated at 135°C for 2h;

[0057] S313, then under mechanical stirring at 120° C., urea was added to the beaker and stirred for 2.5 h to obtain a milky yellow fluid;

[0058] S314, purifying by washing with ethanol precipitation, and finally drying the purified product in an oven at 80° C. to obtain an organic phosphorus-containing flame retardant;

[0059] The synthetic structural formula of organic phosphorus-containing flame retardant is as follows:

[0060]

[0061] In this embodiment, the organic phosphorus-containing flame retardant decomposes at high temperature to generate phosphoric acid, which then turns into metaphosphoric acid, and then condenses into polymetaphosphoric acid, thereby phosphorylating and dehydrating the cotton fiber and converting it into carbon, inhibiting the formation of the combustible intermediate levorotatory glucose during the cracking process of the cotton fiber, thereby inhibiting combustion. The phosphorus-containing flame retardant has a gas phase flame retardant mechanism, and the phosphorus-containing free radicals can capture hydrogen free radicals or hydroxyl free radicals to prevent the reaction of chain free radicals. The reaction is as follows: Figure 2 shown.

[0062] Embodiment 2

[0063] refer to Figure 1 , the preparation method of short-chain cationic fluorocarbon surfactant is as follows:

[0064] S321, firstly, adding hexylsulfonyl fluoride to toluene, and stirring magnetically at room temperature, and adding N,N-dimethyl-1,3-propylenediamine dropwise during stirring;

[0065] Among them, a large amount of yellow solid precipitated after N,N-dimethyl-1,3-propylenediamine was added dropwise, and the stirring method adopted mechanical stirring to ensure sufficient stirring;

[0066] S322, then continue to react under magnetic stirring overnight at room temperature and filter, wash the filter cake with toluene, water and ethanol in turn and dry to obtain a light yellow solid;

[0067] S323, then adding potassium iodide to butanone, adding 1-chloropinacolone after magnetic stirring for 5 minutes, stirring the reaction for 3 hours and filtering;

[0068] S324, washing the filter cake with ethanol and then using 50°C rotary evaporation until there is no fraction, then adding ethanol and the light yellow solid obtained in the reaction of S32, and reflux reaction for 6h;

[0069] S325, finally cooling to room temperature and rotary evaporating until no fraction is left to obtain a red viscous solid short-chain cationic fluorocarbon surfactant;

[0070] The reaction process of the short-chain fluorocarbon surfactant is as follows:

[0071]

[0072] In this embodiment, the addition of the cationic fluorocarbon surfactant effectively reduces the surface tension of the fire extinguishing agent solution and increases the surface activity, so that the fire extinguishing agent can spread on the surface of the burning object after being sprayed. At the same time, the cationic fluorocarbon surfactant also serves as a foaming agent. The dual effects of foam and gel film make fire extinguishing more efficient.

[0073] The following table shows the physical and chemical experimental data of the fire extinguishing agent after adding cationic fluorocarbon surfactant:

[0074] Serial number performance parameter 1 Foaming 169cm 2 Surface tension 24mN / N 3 Viscosity 21254mpa.s 4 pH 7.2

[0075] S4. Finally, the mixed liquids are mixed and stirred for 3 hours, and the pH value is tested. The pH value needs to be maintained within the medium range. The pH can be adjusted to neutral by using a pH adjuster to obtain a special fire extinguishing agent;

[0076] Specifically, the pH value test is used to monitor whether the product is qualified. The pH value test is carried out using pH test paper, or a professional pH test instrument can be used to complete the test. The specific steps for using pH test paper for testing are as follows:

[0077] S41. Place the fire extinguishing agent to be tested into a container;

[0078] S42. Place the pH test paper in the fire extinguisher and take it out after 2 to 3 seconds;

[0079] S43, waiting for the pH test paper to change color and then comparing it with the color comparison card to determine the pH;

[0080] The pH value of the fire extinguishing agent can be adjusted by a pH adjuster to control the pH value within a range of 6.5 to 7.5 to ensure the stability and performance of the fire extinguishing agent.

[0081] Wherein, a dust-free stirring device is used in all stirring steps from S1 to S4 to prevent the fire extinguishing agent from being affected by impurities and pollutants, thereby ensuring the purity and quality of the fire extinguishing agent.

[0082] In addition, the stirring speed in all stirring steps in S1-S4 is between 100 and 300 rpm. This stirring speed range ensures uniform mixing of the components of the fire extinguishing agent, thereby improving the overall performance and quality of the fire extinguishing agent.

[0083] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing a special fire extinguishing agent for textiles, characterized in that: The following steps are involved: S1, adding gluconolactone GDL and calcium carbonate into water, wherein the addition percentages of water, gluconolactone and calcium carbonate are 10%, 2% and 1% respectively, and stirring and dissolving at a constant temperature of 45° C. for 1 hour to obtain a first mixed solution; S2, adding 20% ​​water to the first mixed solution, and then adding lignin and hydroxyethyl cellulose, wherein the addition percentage of lignin and hydroxyethyl cellulose is 3%, and then stirring and dissolving at a constant temperature of 45° C. for 2 hours to obtain a second mixed solution; S3, adding an organic phosphorus-containing flame retardant, a short-chain cationic fluorocarbon surfactant, a preservative and water to the second mixed liquid, wherein the addition percentages of the organic phosphorus-containing flame retardant, the short-chain cationic fluorocarbon surfactant and the preservative are 10%, 2% and 1% respectively, and the remaining 48% is water; S4. Finally, stir for 3 hours and test the pH value. Use a pH adjuster to adjust the pH to neutral to obtain a special fire extinguishing agent.

2. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The preparation method of the organic phosphorus-containing flame retardant in S3 is as follows: S311. First, add bis(2-hydroxyethyl)amino(trihydroxymethyl)methane and phosphoric acid into a beaker equipped with a mechanical stirrer and a thermometer; S312, then heated at 135°C for 2h; S313, then under mechanical stirring at 120° C., urea was added to the beaker and stirred for 2.5 h to obtain a milky yellow fluid; S314, purifying by washing with ethanol precipitation, and finally drying the purified product in an oven at 80° C. to obtain an organic phosphorus-containing flame retardant.

3. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The preparation method of the short-chain cationic fluorocarbon surfactant in S3 is as follows: S321, firstly add all-hexylsulfonyl fluoride to toluene, and stir magnetically at room temperature, and dropwise add N,N-dimethyl-1,3-propanediamine; S322, then continue to react under magnetic stirring overnight at room temperature and filter, wash the filter cake with toluene, water and ethanol in turn and dry to obtain a light yellow solid; S323, then adding potassium iodide to butanone, adding 1-chloropinacolone after magnetic stirring for 5 minutes, stirring the reaction for 3 hours and filtering; S324, washing the filter cake with ethanol and then using 50°C rotary evaporation until there is no fraction, then adding ethanol and the light yellow solid obtained in the reaction of S32, and reflux reaction for 6h; S325. Finally, cool to room temperature and evaporate until there is no fraction, to obtain a red viscous solid short-chain cationic fluorocarbon surfactant.

4. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: A dust-free stirring device is used in all stirring steps from S1 to S4.

5. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The stirring speed in all the stirring steps in S1-S4 is between 100 and 300 rpm.

6. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The weight ratio of the organic phosphorus-containing flame retardant to the short-chain cationic fluorocarbon surfactant in S3 is controlled to be 5:1 to 10:

1.

7. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The pH value of the fire extinguishing agent is adjusted within a range of 6.5 to 7.

5.

8. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: Add dropwise in the S321.

9. A large amount of yellow solid precipitated after N,N-dimethyl-1,3-propylenediamine was added, and mechanical stirring was used.

10. The method for preparing a special fire extinguishing agent for textiles according to claim 1, characterized in that: The pH value test in S4 is performed using pH test paper, and the specific steps are: S41. Place the fire extinguishing agent to be tested into a container; S42. Place the pH test paper in the fire extinguisher and take it out after 2 to 3 seconds; S43. Wait for the pH test paper to change color and then compare it with the color comparison card to determine the pH.

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