CN111549530B - Fireproof fabric/hydrogel composite material and preparation method thereof - Google Patents

Fireproof fabric/hydrogel composite material and preparation method thereof Download PDF

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CN111549530B
CN111549530B CN202010474056.6A CN202010474056A CN111549530B CN 111549530 B CN111549530 B CN 111549530B CN 202010474056 A CN202010474056 A CN 202010474056A CN 111549530 B CN111549530 B CN 111549530B
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fabric
hydrogel
fireproof
composite material
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CN111549530A (en
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费佳蕾
张成远
吴红艳
陈钊聪
赵科
王亚丹
杨欣烨
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Nanjing University of Information Science and Technology
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    • D06M14/00Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/08Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
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    • D06M14/02Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
    • D06M14/06Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of animal origin, e.g. wool or silk
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    • D06M14/12Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06M14/08Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
    • D06M14/12Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract

The invention provides a fireproof fabric/hydrogel composite material and a preparation method thereof, the fireproof fabric/hydrogel composite material is prepared by hydrogel and fabric through a wet chemical crosslinking method, wherein the hydrogel comprises the following components: 5.6 to 6.5 portions of ammonium dodecyl sulfate; naCl 2.0-3.0 weight portions; 75.0 to 81.0 weight portions of water; 10.0 to 13.5 weight portions of N, N-dimethylacrylamide; 0.7-0.9 part by weight of octadecyl methacrylate; 0.05-0.1 part of initiator KPS; 0.15-0.4 weight part of accelerant TEMED and 0.5-0.6 weight part of additive. The material can resist high temperature, and the maximum temperature of the surface and the surface contacting with the skin of the material is lower than 100 ℃ under the firing of high-temperature flame, so that the skin is prevented from being burnt, and the fireproof application in the lifesaving field of fireproof blankets, fire-fighting clothing and the like is met.

Description

Fireproof fabric/hydrogel composite material and preparation method thereof
Technical Field
The invention belongs to the field of preparation of high polymer materials, and relates to a fireproof fabric/hydrogel composite material and a preparation method thereof. The technology has wide application prospect in the lifesaving field of fire blankets, fire-fighting clothing and the like.
Background
Millions of people suffer burns every year around the world. Of these accidents, about 72% of burns occur at home. There is also a great risk of injury when a fire occurs in a small space such as a high-rise building, a ship, or an airplane.
Thus providing inexpensive and effective fire protection devices, such as fire blankets, which can save many lives, there is a great demand for fire-resistant fabrics. The fabric can survive in high temperature fires for a long period of time and protect the skin from burns.
Over the last several decades, significant progress has been made in the development of flame retardant fabrics. Fire resistant fabrics are typically made from fire resistant materials that rely on many different flame retardant mechanisms, including high decomposition temperatures, low thermal conductivity, and carbonization. Existing fire-blocking fabrics suffer from several disadvantages, such that these highly engineered fabrics are expensive, decompose rapidly, and become very hot at high temperatures.
Disclosure of Invention
The present invention provides a fire-resistant fabric/hydrogel composite material having low thermal conductivity and fire-resistant properties.
It is another object of the present invention to provide a method for preparing the above fire-resistant fabric/hydrogel composite, which comprises compounding a fabric with a hydrogel through chemical crosslinking by virtue of the high water content of the hydrogel material to form a fabric/hydrogel composite.
In order to realize the purpose, the technical scheme provided by the invention is as follows:
a fireproof fabric/hydrogel composite material is prepared by performing a wet chemical crosslinking method on hydrogel and fabric, wherein the hydrogel comprises the following components:
5.6 to 6.5 portions of ammonium dodecyl sulfate;
NaCl 2.0-3.0 weight portions;
75.0 to 81.0 weight portions of water;
10.0 to 13.5 weight portions of N, N-dimethylacrylamide;
0.7-0.9 part by weight of octadecyl methacrylate;
0.05 to 0.1 weight portion of initiator KPS;
0.15-0.4 weight of accelerating agent TEMED;
0.5 to 0.6 weight portion of additive.
Preferably, the initiator is water-soluble potassium persulfate KPS.
Preferably, the accelerant is Tetramethylethylenediamine (TEMED).
Preferably, the additive is selected from graphene, titanium nitride or zirconium oxide.
Preferably, the fabric is cotton, hemp, wool, silk, terylene, viscose, spandex or chinlon fabric.
The preparation method of the fireproof fabric/hydrogel composite material comprises the following preparation processes:
1) Preparing hydrogel: firstly, dissolving an additive, ammonium dodecyl sulfate and NaCl in water at room temperature, adding octadecyl methacrylate, and magnetically stirring in a water bath kettle at 35-40 ℃ for 3-4 hours; adding N, N-dimethylacrylamide, and stirring for reaction for 1-2h; then adding an initiator and an accelerant, uniformly stirring to obtain a fireproof hydrogel solution, and transferring the fireproof hydrogel solution to a glass container for later use;
2) Wet chemical crosslinking: transferring a part of the fireproof hydrogel solution prepared in the step 1) into a mold, controlling the thickness of the fireproof hydrogel solution in the mold to be 1.0-2.5mm, laying the fabric on the hydrogel of the mold, and then coating the fabric with a layer of fireproof hydrogel solution with the thickness of 2.0-3.5 mm; thermally initiating at 50 ℃ and carrying out polymerization reaction for 12-13h to obtain the fireproof fabric/hydrogel composite material.
Preferably, the mold is placed in an ultrasonic cleaning instrument in advance, is subjected to ultrasonic treatment for 10-20 min, is washed clean by deionized water and ethanol, and is dried in a nitrogen atmosphere.
Preferably, the fabric is rinsed clean with deionized water and dried in a nitrogen atmosphere.
The invention also provides application of the fireproof fabric/hydrogel composite material in fireproof materials.
Compared with the prior art, the invention has the following beneficial effects:
1. the fireproof fabric/hydrogel composite material prepared by the invention has the advantages of low production cost, simple preparation and no toxicity, and is easy for large-scale industrial production.
2. The fireproof fabric/hydrogel composite material prepared by the invention can resist high temperature due to the high water content of the hydrogel, and the maximum temperature of the surface and the skin contact surface of the fireproof fabric/hydrogel composite material is lower than 100 ℃ and only about 50 ℃ of the skin contact surface under the burning of high-temperature flame, and is within the temperature range which can be borne by the skin. The skin is prevented from being burnt, and the fire protection application in the life saving fields of fire blankets, fire-fighting clothing and the like is met.
3. The fireproof fabric/hydrogel composite material prepared by the invention can effectively prolong the service time of fabrics, fiber cloth and the like in high-temperature flame.
Drawings
FIG. 1 is a picture of polyester compounded in a hydrogel material;
FIG. 2 is a diagram of a terylene fire-proof experiment;
FIG. 3 is a fire-proof experimental diagram of the terylene/hydrogel composite material;
FIG. 4 is a graph showing the temperature change of the polyester/hydrogel composite material at high temperature burning (also shown in the abstract);
from fig. 4, it can be seen that the maximum temperature of the surface of the fireproof fabric/hydrogel composite material and the skin contact surface were both below 100 ℃ and only about 50 ℃ during the whole experiment.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The first embodiment is as follows:
the preparation process of the fireproof fabric/hydrogel composite material comprises the following steps:
(1) And (4) preparing a fireproof hydrogel solution.
Weighing 0.55g of nano zirconia, 6.0g of Ammonium Dodecyl Sulfate (ADS) and 2.5g of NaCl, dissolving in 78.5g of H2O at normal temperature, adding 0.7g of Stearyl Methacrylate (SMA), and placing in a 35 ℃ water bath kettle for magnetic stirring for 3 hours. 11.5g of N, N-dimethylacrylamide (DMAAm) was added thereto, and the mixture was stirred to react for 1 to 2 hours. Then, 0.05g of initiator KPS and 0.2g of accelerant TEMED are added and stirred uniformly to obtain the fireproof hydrogel solution.
(2) Compounding and molding the hydrogel material and the polyester fabric. Transferring the solution obtained by the reaction into a glass test tube, transferring half of the solution prepared in the step (1) into a square mold (the size of the mold is 5cm multiplied by 5cm, placing the mold in an ultrasonic cleaning instrument for ultrasonic treatment for about 15min, then washing the mold with deionized water and ethanol, drying the mold in nitrogen atmosphere, washing the fabric with deionized water, and drying the fabric in nitrogen atmosphere), injecting hydrogel with the thickness of 2m for the first time, placing the fabric in the mold, and then coating a hydrogel film with the thickness of 3mm on the fabric. Thermally initiating at 50 ℃, and carrying out polymerization reaction for 12 hours to obtain the fireproof fabric/hydrogel composite material.
Example two:
the preparation process of the fireproof fabric/hydrogel composite material comprises the following steps:
(1) And (4) preparing a fireproof hydrogel solution. Weighing 0.6g of nano graphene, 6.5g of Ammonium Dodecyl Sulfate (ADS) and 2.5g of NaCl, dissolving in 76.0g of H2O at normal temperature, adding 0.8g of Stearyl Methacrylate (SMA), and placing in a 35 ℃ water bath kettle for magnetic stirring for 3 hours. 10.5g of N, N-dimethylacrylamide (DMAAm) was added thereto, and the mixture was stirred and reacted for 2 hours. Then 0.06g of initiator KPS and 0.3g of accelerant TEMED are added and stirred uniformly to obtain the fireproof hydrogel solution.
(2) Compounding and molding the hydrogel material and the polyester fabric. Transferring half of the solution prepared in the step (1) into a square mold (the size of the mold is 5cm multiplied by 5cm, placing the mold in an ultrasonic cleaning instrument for about 15min of ultrasound, then washing the mold with deionized water and ethanol, drying the mold in a nitrogen atmosphere, washing the fabric with the deionized water, drying the fabric in the nitrogen atmosphere), injecting hydrogel with the thickness of 2m for the first time, placing the fabric in the mold, and then coating a hydrogel film with the thickness of 3mm on the fabric. Thermally initiating at 50 ℃ and carrying out polymerization reaction for 12h to obtain the fireproof fabric/hydrogel composite material.
Example three:
the preparation process of the fireproof fabric/hydrogel composite material comprises the following steps:
(1) And (4) preparing a fireproof hydrogel solution. The preparation method relates to the preparation of the fireproof hydrogel material, and 0.5g of titanium nitride, 5.8g of Ammonium Dodecyl Sulfate (ADS) and 2.2g of NaCl are weighed and dissolved in 80gH at normal temperature 2 O, 0.85g of Stearyl Methacrylate (SMA) is added, and the mixture is placed in a 35 ℃ water bath to be magnetically stirred for 3 hours. 10.5g of N, N-dimethylacrylamide (DMAAm) was added thereto, and the mixture was stirred and reacted for 1.5 hours. Then 0.1g of initiator KPS and 0.15g of accelerant TEMED are added and stirred evenly to obtain the fireproof hydrogel solution.
(2) Compounding and forming the hydrogel material and the cotton fabric. Transferring half of the solution prepared in the step (1) into a square mold (the size of the mold is 5cm multiplied by 5cm, placing the mold in an ultrasonic cleaning instrument for about 15min of ultrasound, then washing the mold with deionized water and ethanol, drying the mold in a nitrogen atmosphere, washing the fabric with the deionized water, drying the fabric in the nitrogen atmosphere), injecting hydrogel with the thickness of 2m for the first time, placing the fabric in the mold, and then coating a hydrogel film with the thickness of 3mm on the fabric. Thermally initiating at 50 ℃ and carrying out polymerization reaction for 12.5h to obtain the fireproof fabric/hydrogel composite material.
Test example one:
the fire-proof performance test specifically operates as follows:
Figure DEST_PATH_IMAGE001
fixing the terylene on an iron support, burning the terylene by a high-temperature spray gun, and recording the change condition of the terylene under high-temperature flame by a camera. As shown in fig. 2, the terylene burns for about 5s completely under the burning of the high temperature spray gun.
Figure DEST_PATH_IMAGE002
The fireproof fabric/hydrogel composite material prepared in the first example was fixed on an iron support, the polyester/hydrogel composite material was burned with a high-temperature spray gun, the change of the fireproof fabric/hydrogel composite material in high-temperature flame was recorded with a video camera, and the change of the temperature of the surface of the fireproof fabric/hydrogel composite material was recorded with an infrared thermometer (every 15 seconds).
As shown in fig. 3, it can be seen that the fire-proof fabric/hydrogel composite prepared in the first example is still intact for 60s under the burning of the high-temperature spray gun.
As shown in fig. 4, it can be seen that the temperature change curve of the fireproof fabric/hydrogel composite material prepared in the first example under high temperature burning condition shows that the maximum temperature of the surface and the skin contact surface of the fireproof fabric/hydrogel composite material is lower than 100 ℃ and the temperature of the skin contact surface is only about 50 ℃ in the whole experiment process. The flameproof fabric/hydrogel composite of the present invention can be used as a flameproof material.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.

Claims (3)

1. A fireproof fabric/hydrogel composite material is prepared by performing a wet chemical crosslinking method on hydrogel and fabric, wherein the hydrogel comprises the following components: 5.6 to 6.5 weight portions of ammonium dodecyl sulfate; naCl 2.0-3.0 weight portions; 75.0 to 81.0 weight portions of water; 10.0 to 13.5 weight portions of N, N-dimethylacrylamide; 0.7-0.9 part by weight of octadecyl methacrylate; 0.05 to 0.1 weight portion of initiator potassium persulfate; 0.15-0.4 part by weight of accelerant tetramethylethylenediamine; 0.5-0.6 part by weight of additive; the additive is titanium nitride or zirconium oxide; the preparation method of the fireproof fabric/hydrogel composite material comprises the following steps:
(1) Preparing hydrogel: firstly, dissolving an additive, ammonium dodecyl sulfate and NaCl in water at room temperature, adding octadecyl methacrylate, and magnetically stirring in a water bath kettle at 35-40 ℃ for 3-4 hours; adding N, N-dimethylacrylamide, and stirring to react for 1-2h; then adding an initiator and an accelerating agent, uniformly stirring to obtain a fireproof hydrogel solution, and transferring the fireproof hydrogel solution to a glass container for later use;
(2) Wet chemical crosslinking: transferring a part of the fireproof hydrogel solution prepared in the step (1) into a mold, controlling the thickness of the fireproof hydrogel solution in the mold to be 1.0-2.5mm, laying the fabric on the hydrogel of the mold, and coating the fabric with a layer of fireproof hydrogel solution with the thickness of 2.0-3.5 mm; thermally initiating at 50 ℃, and carrying out polymerization reaction for 12-13h to obtain a fireproof fabric/hydrogel composite material; the fabric is selected from cotton, hemp, wool, silk, terylene, viscose, spandex or chinlon fabric.
2. The flameproof fabric/hydrogel composite material according to claim 1, wherein in the step (2), the mold is placed in an ultrasonic cleaning apparatus in advance, is subjected to ultrasonic treatment for 10-20 min, is washed clean by deionized water and ethanol, and is dried in a nitrogen atmosphere.
3. The flameproof fabric/hydrogel composite material according to claim 2, wherein in step (2), the fabric is washed clean with deionized water and dried in a nitrogen atmosphere.
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