Preparation method of infrared stealth nimesh spun flame-retardant cotton fabric

Abstract

The application discloses a preparation method of infrared stealth Nais spinning flame-retardant cotton fabric and belongs to the technical field of materials. The organic / inorganic composite aerogel felt is prepared through freeze-drying and chemical cross-linking methods, the MXene / metal powder / aerogel microsphere infrared stealth coating is constructed on the surface of the Nais spinning fabric through a printing coating finishing method, and then the infrared stealth Nais spinning fabric with heat insulation and low infrared emissivity is prepared by using a physical compounding method. The preparation method is simple and controllable, and the preparation components are green and environmentally friendly. The prepared Nais spinning fabric has the characteristics of flame retardation, heat insulation and low infrared emissivity, and the problems of flammability and high infrared emissivity of the Nais spinning fabric are solved, so the Nais spinning fabric has a good application prospect in the fields of flame retardation, heat insulation and infrared stealth.

Description

TECHNICAL FIELD

[0001] The application relates to a preparation method of an infrared stealth nisso fabric flame-retardant cotton fabric and belongs to the technical field of materials. BACKGROUND

[0002] With the popularization and application of infrared imaging technology in military reconnaissance, heat sources such as battlefield soldiers, military targets and weapon equipment are easily detected and attacked, and their survival is seriously threatened. By constructing a low infrared emissivity camouflage layer on the surface of a single soldier combat uniform and filling the inside with thermal insulation materials, the radiation heat of the uniform can be reduced, the thermal characteristics of the target and the background can be integrated, and the uniform has the characteristics of economy, high efficiency and simple process. However, the material is too thick and heavy, and the wearability is poor. Developing a light and durable aerogel filled fabric is an effective method to reduce the mass of thermal insulation materials and improve the wearability.

[0003] Nisso fabric is a spun silk fabric woven from polyamide filaments, which has the characteristics of flatness, fineness, softness, lightness, firmness, wear resistance, easy washing and quick drying, and is mainly used as a fabric for men's and women's clothing. However, the flammable nature of nisso fabric also poses a serious fire hazard in its application field. Developing a coating with simple process and both flame retardant and infrared stealth functions for the preparation of functional nisso fabric is an effective method to reduce fire hazards and expand the application range of nisso fabric.

[0004] Aerogel is a highly porous solid material with low density and low thermal conductivity, which has a special continuous network of connected pore structure and excellent thermal insulation performance, and is very suitable for preparing thermal insulation textiles. Cellulose, as a natural material, has the advantages of green and renewable, and is a good precursor for preparing aerogel. However, cellulose aerogel usually has poor mechanical properties and is highly flammable, which seriously limits its practical application.

[0005] MXene is a new type of two-dimensional nanomaterial, and its general formula is MX n+1 X n T x , wherein T x is a functional group (-OH, -F, -O, etc.) attached to the surface of MXene generated from etching precursors, which has high electrical conductivity and large specific surface area, as well as excellent thermal camouflage performance, and has broad application prospects in the field of infrared camouflage. Most metal materials have low infrared emissivity at low temperature and without surface oxidation, and the emissivity will further decrease after surface polishing treatment, so using metal as the main material to prepare the coating can achieve the purpose of inhibiting the infrared radiation of the object. The composite of MXene and metal powder can be used to prepare a coating material with extremely low infrared emissivity, which has broad application prospects in the field of infrared stealth. SUMMARY

[0006] [Technical Problem] [Technical Solution]

[0007] The technical problem to be solved by the present application is that the single soldier combat uniform is heavy and has poor performance, and the textile fabric using cellulose aerogel cannot simultaneously have flame-retardant and infrared stealth functions, which limits the practical application.

[0008] [Technical Solution]

[0009] In order to solve the above problems, the present application adopts a freeze-drying method to prepare strong and tough flame-retardant organic / inorganic composite aerogel felt and organic / inorganic composite aerogel microspheres, uses a printing coating finishing method to prepare a MXene@(Al / Cu / Ag)@aerogel microsphere low infrared emissivity coating on the surface of a nis textile fabric, and further designs and prepares an infrared stealth nis spunlaced flame-retardant cotton fabric with heat insulation and infrared stealth performance, which can simultaneously realize fabric heat insulation, lightweight, difficult combustion and low infrared emissivity. The fabric preparation method is simple and repeatable, and has good flame-retardant performance and infrared stealth performance.

[0010] The first object of the present application is to provide a preparation method of an infrared stealth nis spunlaced flame-retardant cotton fabric, comprising the following steps:

[0011] (1) Dissolve an organophosphorus monomer in an organic solvent, dropwise add an aminosiloxane, stir under water bath heating conditions for 5-8 hours, remove the solvent, and prepare a halogen-free flame-retardant crosslinking agent;

[0012] (2) Soak the cotton fabric in a flame retardant aqueous solution and stand still, and then dry after taking out, to prepare a flame-retardant cotton fabric;

[0013] (3) Add cellulose to water to prepare a cellulose water dispersion liquid with a concentration of 1-6 mg / g;

[0014] (4) Add the halogen-free flame-retardant crosslinking agent obtained in step (1) to the cellulose water dispersion liquid, heat in a water bath, and ultrasonically stir for 5-8 hours, then place in a vacuum oven and stand still for 6-12 hours to obtain a mixed dispersion liquid; freeze the mixed dispersion liquid using liquid nitrogen, place in a vacuum freeze dryer for freeze-drying, to prepare a strong and tough flame-retardant organic / inorganic composite aerogel felt; transfer the mixed dispersion liquid to a syringe, inject into liquid nitrogen to form frozen microspheres, and place in a vacuum freeze dryer for freeze-drying, to prepare organic / inorganic composite aerogel microspheres;

[0015] (5) Selectively etch Ti3AlC2 with hydrochloric acid and lithium fluoride, collect the precipitate, disperse the precipitate in deionized water, ultrasonically shake, collect the upper suspension and vacuum dry, to obtain 2D Ti3C2T x nanosheets; wherein T x is a surface end group, containing a hydroxyl group, fluorine, oxygen or a combination thereof;

[0016] (6) the organic / inorganic composite aerogel microspheres obtained in step (4), the Ti3C2T x The nanosheet, metal powder and water-based adhesive are added into water, stirred uniformly to prepare a low-infrared emissivity coating agent; the low-infrared emissivity coating slurry is coated on the surface of a base fabric by using a printing coating finishing method to prepare a low-infrared emissivity fabric.

[0017] (7) the flame-retardant cotton fabric obtained in step (2), the strong and tough flame-retardant organic / inorganic composite aerogel felt obtained in step (4) and the low-infrared emissivity fabric obtained in step (6) are sewn to prepare an infrared stealth nispanse flame-retardant cotton fabric.

[0018] In one embodiment of the present application, the organic phosphorus monomer in step (1) is one or more of hexachlorocyclotriphosphazene, phosphorus oxychloride, spirocyclic pentaerythritol diphosphonic dichloride; the aminosiloxane is one or more of 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, piperazine methyl trimethoxysilane and piperazine methyl triethoxysilane; the organic solvent is one of acetonitrile, dimethyl sulfoxide, tetrahydrofuran and N,N-dimethylformamide; and the water bath heating reaction temperature ranges from 50 to 80℃.

[0019] In one embodiment of the present application, the flame retardant in step (2) is one or more of ammonium polyphosphate, tributyl phosphate, triphenyl phosphate, methyl phosphonate dimethyl and triphenyl phosphite.

[0020] In one embodiment of the present application, the cellulose in step (3) is one or more of nanocellulose, bacterial cellulose and cellulose acetate.

[0021] In one embodiment of the present application, the mass ratio of the flame-retardant crosslinking agent to the cellulose in step (4) is (0.1-0.5):1; the inner diameter of the needle of the syringe is 0.05-0.5mm, and the injection rate is 0.5-2mL / min.

[0022] In one embodiment of the present application, the metal powder in step (6) is one or more of aluminum powder, copper powder and silver powder; and the water-based adhesive is one or more of methacrylic acid, ethyl acrylic acid, epoxy resin and polyurethane.

[0023] In one embodiment of the present application, the concentration of the organic / inorganic composite aerogel microspheres in step (6) is 2-5mg / g, and the concentration of the Ti3C2T x The concentration of the nanosheet is 3-10mg / g, and the concentration of the metal powder is 1-10mg / g; and the base fabric is a nispanse fabric.

[0024] In an embodiment of the present application, the thickness of the toughened and flame-retardant organic / inorganic composite aerogel felt in step (7) is 0.3-1.5 mm.

[0025] A second object of the present application is to provide an infrared stealth non-woven spun flame-retardant cotton fabric prepared by the above-mentioned method.

[0026] The present application also provides the application of the above-mentioned infrared stealth non-woven spun flame-retardant cotton fabric in the field of flame retardation, heat insulation and infrared stealth.

[0027] The present application has the following advantages:

[0028] (1) The present application prepares an organic / inorganic composite aerogel felt by freeze-drying and chemical cross-linking, constructs an MXene / metal powder / aerogel microsphere infrared stealth coating on the surface of the non-woven spun fabric by the method of printing and coating finishing, and then uses the method of physical compounding to prepare an infrared stealth non-woven spun fabric with heat insulation and low infrared emissivity. This method is simple, efficient, highly reproducible and environmentally friendly, and has good application prospects in the field of flame retardation, heat insulation and infrared stealth.

[0029] (2) The toughened and flame-retardant aerogel felt of the present application effectively plays the synergistic effect of the double network structure of cellulose aerogel and halogen-free flame-retardant cross-linking agent. The thermal conductivity of the infrared stealth non-woven spun flame-retardant cotton fabric prepared by the aerogel designed by the present application is reduced to 0.04 W·m -1 ·K -1 Hereinafter, the temperature difference with the background temperature under the heating of a 90℃ hot stage reaches 50℃ or more, and the temperature difference under the background of-100℃ liquid nitrogen reaches 55℃ or more.

[0030] (3) The MXene / metal powder / aerogel microsphere infrared stealth coating of the present application effectively plays the low infrared emissivity effect of MXene / metal powder and the heat insulation function of aerogel microspheres, and the infrared emissivity is reduced to below 0.4. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 The reaction equation diagram of the flame-retardant cross-linking agent obtained in Example 1;

[0032] Figure 2 The Fourier infrared (FTIR) diagram of the flame-retardant cross-linking agent obtained in Example 1;

[0033] Figure 3 The scanning electron microscope (SEM) diagram of the toughened and flame-retardant cellulose aerogel felt obtained in Example 1;

[0034] Figure 4 The scanning electron microscope (SEM) diagram of the aerogel microspheres obtained in Example 1;

[0035] Figure 5 Transmission electron microscope (TEM) image of the aerogel microspheres obtained in Example 1;

[0036] Figure 6 Scanning electron microscope (SEM) image of the infrared stealth coating nitspun fabric obtained in Example 1;

[0037] Figure 7 Thermal infrared imaging image of the infrared stealth nitspun flame-retardant cotton fabric obtained in Example 1 under a 90℃ heating environment;

[0038] Figure 8 Thermal infrared imaging image of the infrared stealth nitspun flame-retardant cotton fabric obtained in Example 1 under a human body background;

[0039] Figure 9 Temperature difference curve of the nitspun flame-retardant cotton fabric and the infrared stealth nitspun flame-retardant cotton fabric obtained in Example 1 under a 90℃ heating environment;

[0040] Figure 10 Structural schematic diagram of the infrared stealth nitspun flame-retardant cotton fabric obtained in Example 1. DETAILED DESCRIPTION

[0041] Test method: The surface morphology is observed by a scanning electron microscope; the thermal conductivity coefficient is measured by a thermal conductivity instrument; the heat insulation performance is measured by an infrared thermal imager; and the infrared emissivity is measured by a far infrared emissivity tester.

[0042] Example 1

[0043] (1) 1.044 g of hexachlorocyclotriphosphazene was dissolved in 100 mL of tetrahydrofuran, and 4.015 g of 3-aminopropyltriethoxysilane was slowly added dropwise under a nitrogen atmosphere. After reaction at 65℃ for 3 h, the solvent was removed by rotary evaporation to obtain a halogen-free flame-retardant crosslinking agent;

[0044] (2) 15 g of ammonium polyphosphate was weighed and added to 100 mL of deionized water, and the cotton fabric was soaked in the above solution for 15 minutes and then dried in a 90℃ oven to obtain a flame-retardant cotton fabric;

[0045] (3) 1 g of nanocellulose powder was weighed and added to 200 mL of deionized water, and ultrasonic stirring was performed for 5 hours to obtain a nanocellulose water dispersion solution with a concentration of 5 mg / g;

[0046] (4) Take 15 mg of the above halogen-free flame-retardant crosslinking agent and add it to 10 g of the above nanocellulose dispersion liquid, heat in a water bath at 60 DEG C, and ultrasonically stir for 5 hours, defoam in a vacuum oven for 10 hours, to obtain a mixed dispersion liquid; after the above mixed dispersion liquid is frozen on the surface of a low-temperature mold using liquid nitrogen, it is placed in a vacuum freeze dryer to be freeze-dried, to prepare a 1 mm thick tough flame-retardant organic / inorganic composite aerogel felt; the above mixed dispersion liquid is transferred to a syringe, a spinning needle with an inner diameter of 1 mm is used to inject it into liquid nitrogen at a rate of 1 mL / min to form frozen microspheres, which are placed in a vacuum freeze dryer to be freeze-dried, to prepare organic / inorganic composite aerogel microspheres;

[0047] (5) Add 2 g of lithium fluoride to 40 mL of 19M hydrochloric acid, react at room temperature for 30 min, then raise the temperature to 35 DEG C, add 2 g of Ti3AlC2, react for 24 h, centrifuge, wash with water until the pH is about 7, ultrasonically stir for 60 min, collect the supernatant, and freeze-dry to obtain Ti3C2T x monolayer nanosheet;

[0048] (6) Ultrasonically disperse 45 mg of aluminum powder, 45 mg of Ti3C2T x nanosheet, 30 mg of organic / inorganic composite aerogel microspheres, and 100 mg of methacrylic acid in 15 mL of water, to obtain a uniform low-infrared-emissivity coating agent; use a printing coating finishing method to coat the coating on the surface of a nisshin textile fabric using a coating roller, to obtain a low-infrared-emissivity infrared stealth nisshin textile fabric;

[0049] (7) Stitch the flame-retardant cotton fabric obtained in step (2), the 1 mm thick tough flame-retardant organic / inorganic composite aerogel felt, and the low-infrared-emissivity infrared stealth nisshin textile fabric into a sandwich structure fabric, to prepare an infrared stealth nisshin flame-retardant cotton fabric.

[0050] The reaction equation of the above halogen-free flame-retardant crosslinking agent is shown in Figure 1 ; the above obtained halogen-free flame-retardant crosslinking agent is tested by FTIR, as shown in Figure 2 , the characteristic peaks at 2972, 2883 cm -1 are of ethyl groups, the characteristic peak at 1389 cm -1 is of N-H bonds, the characteristic peak at 1071 cm -1 is of C-O bonds, the characteristic peak at 952 cm -1 is of Si-O bonds, and the characteristic peak at 763 cm -1 is of P-N bonds, which proves that the halogen-free flame-retardant crosslinking agent is successfully prepared.

[0051] The above obtained infrared stealth nisshin flame-retardant cotton fabric is subjected to scanning electron microscope, thermal conductivity, infrared emissivity, and heat insulation performance tests, as shown in Figures 3-9 , and the specific performance results are shown in Table 1.

[0052] Table 1 Performance data of the nisshiki fabric and the infrared stealth nisshiki flame-retardant cotton fabric of Example 1

[0053]

[0054] The preparation method is simple and controllable, the flame-retardant crosslinking agent used is green and environmentally friendly, the infrared stealth nisshiki flame-retardant cotton fabric prepared has good heat insulation performance and low infrared emissivity, and has good infrared stealth performance.

[0055] Example 2

[0056] Preparation of infrared stealth nisshiki flame-retardant cotton fabric with different amounts of aluminum powder

[0057] Referring to Example 1, only the amount of aluminum powder is replaced from 45 mg to 15 mg, 30 mg, 60 mg, and 75 mg respectively, and other conditions remain unchanged, to prepare the infrared stealth nisshiki flame-retardant cotton fabric.

[0058] The performance of the obtained infrared stealth nisshiki flame-retardant cotton fabric is determined, and the results are shown in Table 2.

[0059] Table 2 Performance data of infrared stealth nisshiki flame-retardant cotton fabric prepared with different amounts of aluminum powder

[0060]

[0061] It can be seen that, with other conditions remaining unchanged, the amount of aluminum powder is increased, the infrared emissivity is reduced, and the thermal conductivity is slightly improved, but when the amount of aluminum powder exceeds 45 mg, the reduction in infrared emissivity is significantly reduced.

[0062] Example 3

[0063] Preparation of infrared stealth nisshiki flame-retardant cotton fabric with different thicknesses of tough flame-retardant organic / inorganic composite aerogel felt

[0064] Referring to Example 1, only the thickness of the tough flame-retardant organic / inorganic composite aerogel felt is replaced from 1 mm to 0.3 mm, 0.5 mm, 0.8 mm, 1.2 mm, and 1.5 mm respectively, and other conditions remain unchanged, to prepare the infrared stealth nisshiki flame-retardant cotton fabric.

[0065] The performance of the obtained infrared stealth nisshiki flame-retardant cotton fabric is determined, and the results are shown in Table 3.

[0066] Table 3 Performance data of infrared stealth nisshiki flame-retardant cotton fabric prepared with different thicknesses of tough flame-retardant organic / inorganic composite aerogel felt

[0067]

[0068] It can be seen that, with other conditions unchanged, the thickness of the tough flame-retardant organic / inorganic composite aerogel felt increases, the infrared emissivity is basically unchanged, and the thermal conductivity decreases, but the fabric thickness increases.

[0069] Example 4

[0070] Different celluloses for preparing infrared stealth nimesi flame-retardant cotton fabric

[0071] Referring to Example 1, only the nanocellulose is replaced by bacterial cellulose and cellulose acetate respectively, and other conditions are unchanged, to prepare infrared stealth nimesi flame-retardant cotton fabric.

[0072] The performance of the obtained infrared stealth nimesi flame-retardant cotton fabric is determined, and the results are shown in Table 4.

[0073] Table 4 Performance data of infrared stealth nimesi flame-retardant cotton fabric prepared by different celluloses

[0074]

[0075] It can be seen that, with other conditions unchanged, the infrared stealth nimesi flame-retardant cotton fabric prepared by bacterial cellulose and cellulose acetate has slightly increased thermal conductivity, reduced heat insulation performance, and basically unchanged infrared emissivity.

[0076] Example 5

[0077] Different metal powders for preparing infrared stealth nimesi flame-retardant cotton fabric

[0078] Referring to Example 1, only the aluminum powder is replaced by copper powder and silver powder respectively, and other conditions are unchanged, to prepare infrared stealth nimesi flame-retardant cotton fabric.

[0079] The performance of the obtained infrared stealth nimesi flame-retardant cotton fabric is determined, and the results are shown in Table 5.

[0080] Table 5 Performance data of infrared stealth nimesi flame-retardant cotton fabric prepared by different metal powders

[0081]

[0082] It can be seen that, with other conditions unchanged, the infrared stealth nimesi flame-retardant cotton fabric prepared by copper powder has slightly increased thermal conductivity and infrared emissivity, and the infrared stealth nimesi flame-retardant cotton fabric prepared by silver powder has slightly increased thermal conductivity and reduced infrared emissivity.

[0083] Although the present application has been disclosed with reference to the preferred embodiments as above, it is not limited thereto, and any person skilled in the art can make various modifications, replacements and modifications without departing from the principles and spirits of the present application, and therefore the protection scope of the present application should be defined by the claims.

Claims

1. A process for the preparation of an infrared cloaking nysfing flame resistant cotton fabric characterized in that, It comprises the following steps: (1) Dissolve the organophosphorus monomer in the organic solvent, drop the aminosiloxane, stir and react under the condition of water bath heating, to prepare the halogen-free flame-retardant crosslinking agent; (2) Soak the cotton fabric in the aqueous solution of the flame retardant, and dry after taking out, to prepare the flame-retardant cotton fabric; (3) Add the cellulose into water to prepare the cellulose aqueous dispersion with the concentration of 1-6 mg / g; (4) Add the halogen-free flame-retardant crosslinking agent obtained in step (1) into the cellulose aqueous dispersion of step (3), heat in water bath, stir under ultrasonic, and then place in the vacuum oven for 6-12 hours to obtain the mixed dispersion; freeze the mixed dispersion using liquid nitrogen, and freeze dry in the vacuum freeze dryer to prepare the tough flame-retardant organic / inorganic composite aerogel felt; transfer the mixed dispersion into the syringe, inject into the liquid nitrogen to form the frozen microspheres, and freeze dry in the vacuum freeze dryer to prepare the organic / inorganic composite aerogel microspheres; (5) Ti3AlC2 is selectively etched with hydrochloric acid and lithium fluoride, the precipitate is collected and separated, the precipitate is dispersed in deionized water, ultrasonic oscillation is performed, the upper suspension is collected and vacuum dried to obtain 2D Ti3C2T x nanosheets; wherein, T x is a surface end group, comprising a hydroxyl group, fluorine, oxygen or a combination thereof; (6) the organic / inorganic composite aerogel microspheres obtained in step (4) and the Ti3C2T x The nano sheet, metal powder and water-based binder are added into water, stirred uniformly to prepare a low infrared emissivity coating agent; the low infrared emissivity coating slurry is coated on the surface of the Niss textile fabric by using the printing coating after-finishing mode to prepare a low infrared emissivity fabric; the concentration of the metal powder is 2.96-10 mg / g; (7) Sew the flame-retardant cotton fabric obtained in step (2), the tough flame-retardant organic / inorganic composite aerogel felt obtained in step (4), and the low infrared emissivity fabric obtained in step (6) to prepare the infrared stealth nisshin paste flame-retardant cotton fabric.

2. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, The organophosphorus monomer in step (1) is one or more of hexachlorocyclotriphosphazene, phosphorus oxychloride, and spirocyclic pentaerythritol diphosphate dichlorophosphate; the aminosiloxane is one or more of 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, piperazine methyl trimethoxysilane, and piperazine methyl triethoxysilane; the organic solvent is one of acetonitrile, dimethyl sulfoxide, tetrahydrofuran, and N,N-dimethylformamide; and the water bath heating reaction temperature ranges from 50 to 80℃.

3. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, The flame retardant in step (2) is one or more of ammonium polyphosphate, tributyl phosphate, triphenyl phosphate, methyl phosphonate dimethyl, and triphenyl phosphite.

4. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, The cellulose in step (3) is one or more of nanocellulose, bacterial cellulose, and cellulose acetate.

5. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, In step (4), the mass ratio of the halogen-free flame-retardant crosslinking agent to the cellulose is (0.1-0.5):1; the inner diameter of the needle of the syringe is 0.05-0.5 mm, and the injection rate is 0.5-2 mL / min.

6. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, In step (6), the metal powder is one or more of aluminum powder, copper powder, and silver powder; and the water-based adhesive is one or more of methacrylic acid, ethyl acrylic acid, epoxy resin, and polyurethane.

7. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, In step (6), the concentration of aerogel microspheres is 2-5 mg / g, Ti3C2T x The concentration of nanosheets is 3-10 mg / g.

8. A process for the preparation of an infrared stealth nish-paste flame resistant cotton fabric as claimed in claim 1, wherein, In step (7), the thickness of the tough flame-retardant organic / inorganic composite aerogel felt is 0.3-1.5 mm.

9. An infrared stealth nisshin paste flame-retardant cotton fabric prepared by the method of any one of claims 1-8.

10. The application of the infrared stealth nisshin paste flame-retardant cotton fabric of claim 9 in the field of flame retardation, heat insulation, and infrared stealth.

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