Multi-spectrum composite profiling camouflage material and processing method thereof

Abstract

The invention discloses a multi-spectrum composite profiling camouflage material and a processing method thereof, and belongs to the technical field of profiling camouflage material preparation. The multi-spectrum composite profiling camouflage material comprises a PU hydrophobic matrix layer, an infrared reflection layer, a transition layer, an absorbing layer and a camouflage layer in sequence, wherein the PU hydrophobic matrix layer material is prepared from PU stone and hydrophobic organic matter; the infrared reflection layer material is prepared from distilled water, nano titanium dioxide, silicon dioxide, a dispersant, a defoaming agent and a binder; the transition layer material is prepared from epoxy resin and aluminum powder; the absorbing layer material is prepared from m-bromoacetophenone, thiophene-2-formaldehyde, nitromethane, ammonium acetate, N,N-diisopropylethylamine, N-bromosuccinimide and chopped carbon fiber; the camouflage layer material is composed of camouflage pigment and nylon. The profiling camouflage material prepared by the method has excellent waterproof and shielding properties.

Description

Technical Field

[0001] The invention belongs to the technical field of camouflage material preparation, and in particular relates to a multi-spectrum composite profiling camouflage material and a processing method thereof. Background Art

[0002] Traditional stealth materials, such as radar absorbing materials and camouflage coatings, can only respond to detection of specific frequencies, making it difficult to achieve comprehensive stealth effects. Therefore, it is particularly important to develop a camouflage material that can simultaneously respond to multiple detection methods and achieve multi-frequency compatible stealth effects.

[0003] The Chinese invention patent application with publication number CN111909657B discloses a profiling multi-spectrum composite camouflage material and its preparation method, which sequentially comprises an inner layer substrate, an infrared reflection layer, a transition layer, an outer layer substrate, a profiling absorbing layer and a camouflage layer, wherein the profiling absorbing layer is a polyurethane foam body with an absorbent and a camouflage pigment added thereto, and the surface of the profiling absorbing layer can simulate the contour of the surrounding environment or a specific target. The camouflage material of the invention meets the requirements of multi-spectrum compatibility, can achieve a camouflage effect compatible with visible light, infrared and radar multi-bands, and can imitate the surrounding environment or a specific target, and has a profiling function, but the waterproof performance and shielding performance of the camouflage material prepared by this method still have room for improvement. Summary of the invention

[0004] The object of the present invention is to provide a multi-spectrum composite contour camouflage material and a processing method thereof, so as to solve the technical problem of poor waterproof performance and shielding performance of camouflage materials in the prior art.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The invention provides a multi-spectrum composite profiling camouflage material, which comprises a PU hydrophobic matrix layer, an infrared reflection layer, a transition layer, an absorbing layer and a camouflage layer in sequence, wherein the PU hydrophobic matrix layer material is prepared from PU stone and hydrophobic organic matter; the infrared reflection layer material is prepared from distilled water, nano titanium dioxide, silicon dioxide, a dispersant, a defoaming agent and a binder; the transition layer material is prepared from epoxy resin and aluminum powder; the absorbing layer material is prepared from m-bromoacetophenone, thiophene-2-carboxaldehyde, nitromethane, ammonium acetate, N,N-diisopropylethylamine, N-bromosuccinimide and chopped carbon fiber; and the camouflage layer material is composed of camouflage pigment and nylon.

[0007] Preferably, the method for preparing the PU hydrophobic base layer material comprises the following steps:

[0008] Q1: Add dichloromethylvinylsilane and trimethylmonochlorosilane into a container, mix and stir in an ice-water bath, then slowly add isopropanol to continue the reaction. After the reaction is completed, add deionized water to continue the reaction, then stop stirring, let stand, wash the organic layer, add molecular sieves, filter, and distill under reduced pressure to obtain a colorless transparent liquid;

[0009] Q2: Add a colorless transparent liquid and thioglycolic acid into a container, then add tetrahydrofuran, stir and mix evenly, add benzoin diethyl ether, irradiate with ultraviolet light for reaction, then add perfluorooctylethanol into dichloromethane, stir and add dropwise into the container, react, rotary evaporate, wash, and vacuum dry to obtain a hydrophobic organic substance;

[0010] Q3: The PU stone is placed in acetone and deionized water for ultrasonic cleaning and then dried. The hydrophobic organic matter is then added to the distilled water and ultrasonically stirred to obtain a mixed solution. The dried PU stone is then added to the mixed solution and ultrasonically oscillated. The PU stone is then taken out, washed, and dried to obtain the PU hydrophobic matrix layer material.

[0011] In the above process, the synthesis reaction formula of hydrophobic organic matter is as follows:

[0012]

[0013] The results of mass spectrometry analysis of the colorless and transparent liquid were: m / z: 248.11 (100.0%), 249.11 (25.3%), 250.11 (12.8%), 251.11 (1.2%), 251.10 (1.0%); the results of mass spectrometry analysis of the hydrophobic organic matter were: m / z: 786.10 (100.0%), 787.10 (39.3%), 788.09 (14.6%), 788.10 (7.9%), 789.10(4.1%), 789.09 (1.8%).

[0014] Preferably, in Q1, the dosage ratio of dichloromethylvinylsilane, trimethyl monochlorosilane, isopropanol and deionized water is (2.82-3.67) g: (10.86-14.12) g: (7.2-9.36) g: (3.24-4.21) mL, the mixing time is 10-15 min, the continued reaction time is 30-45 min, the continued reaction time of adding deionized water is 1-2 h, and the standing time is 10-20 min; in Q2, the colorless transparent liquid, thioglycolic acid, tetrahydrofuran, The dosage ratio of benzoin diethyl ether, perfluorooctylethanol and dichloromethane is (2.48-3.72) g: (1.01-1.52) g: (5-7.5) mL: (0.07-0.11) g: (0.53-0.8) g: (7-10.5) mL, the stirring mixing time is 45-60 min, the ultraviolet light wavelength of the ultraviolet irradiation reaction is 320-400 nm, the irradiation time is 15-30 min, the reaction time is 24-36 h, the vacuum drying temperature is 60-70 ° C, and the time is 36-48 h.

[0015] Preferably, in Q3, the ultrasonic cleaning time is 2-4 hours, the usage ratio of PU stone, hydrophobic organic matter and distilled water is (1-2) kg: (100-150) g: (1-2) L, the ultrasonic stirring time is 30-45 min, the ultrasonic oscillation time is 2-3 hours, washing is carried out with distilled water, the drying temperature is 60-70°C, and the time is 3-5 hours.

[0016] Preferably, the method for preparing the wave absorbing layer material comprises the following steps:

[0017] S1: Add m-bromoacetophenone and thiophene-2-carboxaldehyde to a container containing methanol, add potassium hydroxide solution under low temperature, stir at room temperature for reaction, cool, filter, wash, and recrystallize to obtain a light yellow solid; add the light yellow solid, diethylamine, and nitromethane to a container containing methanol, heat under reflux for reaction, cool, acidify, extract, combine the organic phases, dry, concentrate under reduced pressure, and purify to obtain a brown oil;

[0018] S2: Add brown oil and ammonium acetate to a container containing ethanol, heat to reflux under argon protection, cool, wash, and filter to obtain a black solid after reflux. Add the black solid to dichloromethane, stir to dissolve, add N,N-diisopropylethylamine dropwise at low temperature under argon protection, continue stirring, add boron trifluoride etherate dropwise, heat, stir to react, add the mixture to cold water after the reaction is completed, filter, and purify to obtain an intermediate product.

[0019] S3: N-bromosuccinimide and the intermediate product were dissolved in dichloromethane to obtain solution 1 and solution 2, solution 1 was added dropwise to solution 2, and the mixture was stirred to react in the dark, and vacuum evaporated and purified to obtain a yellow-brown solid;

[0020] S4: placing the chopped carbon fiber in a muffle furnace for high-temperature treatment, then taking it out and soaking it in sodium hydroxide solution, drying it to obtain pretreated chopped carbon fiber, adding the yellowish brown solid into dichloromethane, stirring to obtain solution 3, and then adding the pretreated chopped carbon fiber into solution 3, heating and stirring, filtering, and drying to obtain the absorbing layer material.

[0021] In the above process, the synthetic reaction formula of the yellow-brown solid is as follows:

[0022]

[0023] The results of mass spectrometry analysis of the light yellow solid were: m / z: 293.95 (100.0%), 291.96 (98.2%), 292.96 (14.7%), 294.96 (13.6%), 295.95 (4.3%), 294.95 (1.4%), 295.96 (1.2%), 293.96 (1.2%); the results of mass spectrometry analysis of the brown oil were: m / z: 354.97 (100.0%), 352.97(98.1%), 355.97 (16.4%), 353.98 (15.1%), 356.97 (5.2%), 354.98 (1.7%), 353.97(1.1%), 356.98 (1.1%); the results of mass spectrometry analysis of the black solid were: m / z: 618.92 (100.0%), 620.92(55.9%), 616.92 (49.0%), 619.92 (32.9%), 621.92 (18.1%), 617.93 (14.9%),620.93 (4.5%), 622.91 (4.4%), 618.93 (2.4%), 622.93 (2.1%), 623.92 (1.4%),617.92 (1.3%); the results of mass spectrometry analysis of the intermediate products were: m / z: 666.92 (100.0%), 668.92 (59.8%),664.92 (48.8%), 667.92 (46.1%), 665.92 (40.5%), 669.92 (18.5%), 663.92(12.0%), 666.93 (9.3%), 670.91 (4.4%), 668.93 (4.4%), 664.93 (3.7%), 670.92(3.2%), 667.93 (1.6%), 671.92 (1.4%), 669.93 (1.1%); the results of mass spectrometry analysis of the yellow-brown solid were: m / z: 982.56 (100.0%), 984.56 (73.2%), 980.56 (69.5%), 983.56 (47.0%),981.56 (45.5%), 986.55 (30.4%), 978.56 (27.8%), 985.56 (27.8%), 979.56(26.2%), 984.55 (8.0%), 987.56 (7.9%), 977.56 (7.0%), 988.55 (6.5%), 980.57(6.2%), 986.56 (6.1%), 976.56 (4.7%), 987.55 (4.1%), 985.55 (3.3%), 982.57(3.1%), 978.57 (2.3%), 989.55 (2.2%), 988.56 (2.0%), 977.57 (1.5%), 983.57(1.4%), 975.57 (1.2%), 983.55 (1.1%), 985.57 (1.1%), 981.57 (1.1%). .

[0024] Preferably, in S1, the amount ratio of m-bromoacetophenone, thiophene-2-carboxaldehyde, methanol and potassium hydroxide solution is (9.95-14.93) g: (6.73-10.1) g: (250-375) mL: (15-22.5) mL, the low temperature environment temperature is 0-3 ° C, the concentration of potassium hydroxide solution is 2.5 mol / L, the stirring reaction time is 10-12 h, and the mixture is washed with petroleum ether; the light yellow solid, diethylamine, nitromethane and The dosage ratio of methanol is (6.01-8.41) g: (7.32-10.25) g: (6.5-9.1) g: (150-210) mL, the heating reflux temperature is 80-90°C, the reaction time is 10-12h, cooled to 0-1°C, added with 2.5mol / L hydrochloric acid to acidify to pH=2, extracted with dichloromethane, dried with anhydrous sodium sulfate, and purified with a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 10:1.

[0025] Preferably, in S2, the brown oil, ammonium acetate and ethanol are used in a ratio of (1.4-1.68) g: (10.9-13.08) g: (80-96) mL, the heating reflux temperature is 90-95°C, the time is 20-24 h, the reaction mixture is cooled to 0-1°C, and the mixture is washed with petroleum ether; the black solid, dichloromethane, N,N-diisopropylethylamine and boron trifluoride ether are used in a ratio of (0.93-1.21) g: (10-13) mL: (2.5-3.25) mL: (5.67-7.37) mL, the low temperature environment temperature is 0-1°C, the stirring time is 30-45 min, the mixture is heated to room temperature, the stirring reaction time is 48-52 h, and the mixture is purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 2:1.

[0026] Preferably, in S3, the dosage ratio of N-bromosuccinimide and the intermediate product is (0.27-0.49) g: (0.1-0.18) g, the stirring reaction time is 20-24 h, and the mixture is purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 1:2; in S4, the high temperature treatment temperature is 400-450°C, the time is 2-3 h, the concentration of the sodium hydroxide solution is 0.1 mol / L, the soaking time is 2-3 h, the drying temperature is 60-70°C, the time is 10-12 h, the dosage ratio of the yellow-brown solid, dichloromethane and pretreated chopped carbon fiber is (0.4-0.52) g: (5-6.5) mL: (3-3.8) g, the heating and stirring temperature is 70-80°C, and the time is 2-3 h.

[0027] Preferably, the processing method of the multi-spectrum composite profiling camouflage material comprises the following steps:

[0028] Step 1: Mix and stir distilled water, nano titanium dioxide, silicon dioxide, dispersant, defoamer and binder to obtain infrared reflection layer material, mix and stir epoxy resin and aluminum powder to obtain transition layer material, and mix camouflage pigment and nylon to obtain camouflage layer material;

[0029] Step 2: Evenly apply the infrared reflective layer material on the surface of the PU hydrophobic base layer material, then evenly apply the transition layer material on the surface of the infrared reflective layer, then evenly cover the absorbing layer material on the surface of the transition layer, and finally, fix the camouflage layer material on the surface of the absorbing layer by glue. After drying, a multi-spectrum composite contoured camouflage layer material is obtained.

[0030] Preferably, in step 1, the dosage ratio of distilled water, nano titanium dioxide, silicon dioxide, dispersant, defoaming agent and binder is (10-12) mL: (2-3) g: (1-2) g: (0.1-0.3) g: (0.01-0.02) g: (0.2-0.3) g, the mass ratio of epoxy resin to aluminum powder is (8-12): (1-3), and the mass ratio of camouflage pigment to nylon is (3-6): (9-12).

[0031] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0032] 1. The present invention first uses dichloromethylvinylsilane, trimethyl monochlorosilane, thioglycolic acid, and perfluorooctylethanol as raw materials to prepare hydrophobic organic matter, and then compounds the hydrophobic organic matter with PU stone to obtain a PU hydrophobic matrix layer material; then uses m-bromoacetophenone, thiophene-2-carboxaldehyde, nitromethane, ammonium acetate, boron trifluoride etherate, N-bromosuccinimide, and chopped carbon fibers as raw materials to prepare an absorbing layer material, and uses these two materials to prepare a multi-spectrum composite profile camouflage material, which can effectively improve its waterproof performance and shielding performance.

[0033] 2. The present invention uses dichloromethylvinylsilane, trimethyl monochlorosilane, mercaptoacetic acid, and perfluorooctylethanol as raw materials to prepare hydrophobic organic matter, which is compounded with PU stone to obtain a PU hydrophobic matrix layer material. The silicon-oxygen bond contained in the hydrophobic organic matter has a high bond energy, which makes the silicon-oxygen structure stable. At the same time, the silicon-oxygen chain segments are soft and easily deformed after multiple collisions, which helps it to form a stable hydrophobic layer on the surface of the material. The oxygen atoms contained in the silicon-oxygen structure can form hydrogen bonds with water molecules. Due to the softness and steric hindrance effect of the silicon-oxygen chain, the formation of hydrogen bonds is hindered, reducing the contact and adsorption of water molecules with the material surface; and the fluorine atoms contained in the hydrophobic organic matter have extremely strong electronegativity, can strongly attract electron clouds, reduce the surface energy of the fluoride, and have excellent hydrophobic properties. After compounding it with the PU stone, its hydrophobic properties can be effectively improved.

[0034] 3. The present invention uses m-bromoacetophenone, thiophene-2-carboxaldehyde, nitromethane, ammonium acetate, boron trifluoride etherate, N-bromosuccinimide and chopped carbon fibers as raw materials to prepare an absorbing layer material. The obtained yellow-brown solid contains a pyrrole ring. The presence of the pyrrole ring is conducive to the capture and absorption of electromagnetic waves. The bromine atom contained is a heavy atom with excellent electronegativity and polarization ability. The introduction of bromine atoms can change the electron cloud distribution and energy level structure of the molecule, making the molecule more sensitive to electromagnetic waves. The bromine atoms can also serve as electron acceptors to form intramolecular or intermolecular charge transfer complexes with nitrogen atoms on the pyrrole ring, thereby enhancing the absorbing performance of the material and achieving absorption and shielding of electromagnetic waves. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0036] Figure 1 It is a schematic structural diagram of the multi-spectrum composite profiling camouflage material of the present invention.

[0037] Description of the drawings: 1. PU hydrophobic base layer, 2. infrared reflection layer, 3. transition layer, 4. wave absorbing layer, 5. camouflage layer. DETAILED DESCRIPTION

[0038] The technical solutions in the embodiments of the present invention are described clearly and completely below. 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 creative work are within the scope of protection of the present invention.

[0039] Example 1: See Figure 1 As shown, the multi-spectrum composite prosthetic camouflage material comprises a PU hydrophobic matrix layer 1, an infrared reflection layer 2, a transition layer 3, an absorbing layer 4 and a camouflage layer 5 in sequence, wherein the PU hydrophobic matrix layer material is prepared from PU stone and hydrophobic organic matter; the infrared reflection layer material is prepared from distilled water, nano titanium dioxide, silicon dioxide, a dispersant, a defoaming agent and a binder; the transition layer material is prepared from epoxy resin and aluminum powder; the absorbing layer material is prepared from m-bromoacetophenone, thiophene-2-carboxaldehyde, nitromethane, ammonium acetate, N,N-diisopropylethylamine, N-bromosuccinimide and chopped carbon fiber; and the camouflage layer material is composed of camouflage pigment and nylon.

[0040] Embodiment 2: This embodiment discloses a method for preparing a PU hydrophobic matrix layer material, comprising the following steps:

[0041] Q1: 3.25 g of dichloromethylvinylsilane and 12.49 g of trimethylmonochlorosilane were added to a container, mixed and stirred for 15 min in an ice-water bath, and then 8.28 g of isopropanol was slowly added, and the reaction was continued for 45 min. After the reaction was completed, 3.73 mL of deionized water was added dropwise and the reaction was continued for 2 h. Then the stirring was stopped, and the mixture was allowed to stand for 10 min. The organic layer was washed, molecular sieves were added, filtered, and distilled under reduced pressure to obtain a colorless transparent liquid.

[0042] Q2: 3.1 g of colorless transparent liquid and 1.27 g of thioglycolic acid were added to a container, followed by 6.25 mL of tetrahydrofuran, stirred for 60 min, 0.09 g of benzoin diethyl ether was added, and the mixture was irradiated with 365 nm ultraviolet light for 30 min, followed by 0.67 g of perfluorooctylethanol was added to 8.75 mL of dichloromethane, stirred and added dropwise to the container, and the mixture was reacted for 36 h, followed by rotary evaporation, washing, and vacuum drying at 70 ° C for 48 h to obtain a hydrophobic organic compound;

[0043] Q3: 1.5 kg of PU stone was ultrasonically cleaned in acetone and deionized water for 4 hours and then dried. Then 125 g of hydrophobic organic matter was added to 1.5 L of distilled water and ultrasonically stirred for 45 minutes to obtain a mixed solution. Then the dried PU stone was added to the mixed solution and ultrasonically oscillated for 3 hours. The PU stone was then taken out, washed with distilled water, and dried at 70°C for 5 hours to obtain a PU hydrophobic matrix layer material.

[0044] This embodiment discloses a method for preparing an absorbing layer material, comprising the following steps:

[0045] S1: Add 12.44g of m-bromoacetophenone and 8.42g of thiophene-2-carboxaldehyde to a container containing 280mL of methanol, add 18.8mL of 2.5mol / L potassium hydroxide solution at 0℃, stir at room temperature for 12h, cool, filter, wash with petroleum ether, and recrystallize to obtain a light yellow solid; add 7.21g of light yellow solid, 8.71g of diethylamine and 7.8g of nitromethane to a container containing 180mL of methanol, heat under reflux at 90℃ for 12h, cool to 1℃ after the reaction, add 2.5mol / L hydrochloric acid to acidify to pH=2, extract with dichloromethane, combine the organic phases, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 10:1 to obtain a brown oil;

[0046] S2: Add 1.54 g of brown oil and 11.73 g of ammonium acetate to a container containing 88 mL of ethanol, and heat to reflux at 90 ° C for 24 h under argon protection. After the reflux is completed, cool to 0 ° C, wash with petroleum ether, and filter to obtain a black solid; add 1.05 g of black solid to 11.5 mL of dichloromethane, stir to dissolve, and under argon protection, add 2.8 mL of N, N-diisopropylethylamine dropwise at 1 ° C. After stirring for 45 min, add 6.5 mL of boron trifluoride ether, warm to room temperature, and stir to react for 48 h. After the reaction is completed, add the mixture into cold water, filter, and purify with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 2:1 to obtain an intermediate product;

[0047] S3: 0.38 g of N-bromosuccinimide and 0.14 g of the intermediate product were dissolved in 10 mL of dichloromethane to obtain solution 1 and solution 2, and solution 1 was added dropwise to solution 2. The mixture was stirred for 24 h under light-proof conditions, and then evaporated in vacuo. The mixture was purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 1:2 to obtain a yellow-brown solid.

[0048] S4: The chopped carbon fiber was placed in a muffle furnace at 450°C for high temperature treatment for 3 hours, then taken out and soaked in a 0.1 mol / L sodium hydroxide solution for 3 hours, and dried at 60°C for 12 hours to obtain pretreated chopped carbon fiber. 0.46 g of yellowish brown solid was added to 5.5 mL of dichloromethane and stirred to obtain solution 3. Then 3.4 g of pretreated chopped carbon fiber was added to solution 3, heated and stirred at 70°C for 3 hours, filtered and dried to obtain the absorbing layer material.

[0049] This embodiment discloses a method for processing a multi-spectrum composite profiling camouflage material, comprising the following steps:

[0050] Step 1: 11 mL of distilled water, 2.5 g of nano titanium dioxide, 1.5 g of silicon dioxide, 0.2 g of dispersant, 0.015 g of defoamer and 0.25 g of binder are mixed and stirred to obtain an infrared reflection layer material, 10 g of epoxy resin and 2 g of aluminum powder are mixed and stirred to obtain a transition layer material, and 4.5 g of camouflage pigment and 10.5 g of nylon are mixed to obtain a camouflage layer material;

[0051] Step 2: Evenly apply the infrared reflective layer material on the surface of the PU hydrophobic base layer material, then evenly apply the transition layer material on the surface of the infrared reflective layer, then evenly cover the absorbing layer material on the surface of the transition layer, and finally, fix the camouflage layer material on the surface of the absorbing layer by glue. After drying, a multi-spectrum composite contoured camouflage layer material is obtained.

[0052] Embodiment 3: This embodiment discloses a method for preparing a PU hydrophobic matrix layer material, comprising the following steps:

[0053] Q1: Add 2.82g of dichloromethylvinylsilane and 14.12g of trimethylmonochlorosilane into a container, mix and stir for 15min in an ice-water bath, then slowly add 7.2g of isopropanol, and continue to react for 45min. After the reaction is completed, add 3.24mL of deionized water and continue to react for 2h, then stop stirring, let stand for 10min, wash the organic layer, add molecular sieves, filter, and distill under reduced pressure to obtain a colorless transparent liquid;

[0054] Q2: Add 2.48g of colorless transparent liquid and 1.01g of thioglycolic acid to a container, then add 5mL of tetrahydrofuran, stir and mix for 60min, then add 0.07g of benzoin diethyl ether, irradiate with 365nm ultraviolet light for 30min, then add 0.53g of perfluorooctylethanol to 10.5mL of dichloromethane, stir and add dropwise to the container, react for 36h, rotary evaporate, wash, and vacuum dry at 70℃ for 48h to obtain a hydrophobic organic matter;

[0055] Q3: 1kg of PU stone was ultrasonically cleaned in acetone and deionized water for 4 hours respectively, and then dried. Then 100g of hydrophobic organic matter was added to 2L of distilled water and ultrasonically stirred for 45 minutes to obtain a mixed solution. Then the dried PU stone was added to the mixed solution and ultrasonically oscillated for 3 hours. Then the PU stone was taken out, washed with distilled water, and dried at 70°C for 5 hours to obtain the PU hydrophobic matrix layer material.

[0056] This embodiment discloses a method for preparing an absorbing layer material, comprising the following steps:

[0057] S1: Add 9.95g of m-bromoacetophenone and 6.73g of thiophene-2-carboxaldehyde to a container containing 250mL of methanol, add 15mL of 2.5mol / L potassium hydroxide solution at 0℃, stir at room temperature for 12h, cool, filter, wash with petroleum ether, and recrystallize to obtain a light yellow solid; add 6.01g of light yellow solid, 7.32g of diethylamine and 6.5g of nitromethane to a container containing 150mL of methanol, heat under reflux at 90℃ for 12h, cool to 1℃ after the reaction, add 2.5mol / L of hydrochloric acid to acidify to pH=2, extract with dichloromethane, combine the organic phases, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 10:1 to obtain a brown oil;

[0058] S2: Add 1.4 g of brown oil and 10.9 g of ammonium acetate to a container containing 80 mL of ethanol, heat and reflux at 90 ° C for 24 h under argon protection, cool to 0 ° C after reflux, wash with petroleum ether, and filter to obtain a black solid; add 0.93 g of black solid to 10 mL of dichloromethane, stir to dissolve, add 2.5 mL of N, N-diisopropylethylamine dropwise at 1 ° C under argon protection, continue stirring for 45 min, then add 5.67 mL of boron trifluoride ether, warm to room temperature, stir to react for 48 h, and after the reaction is completed, add the mixture into cold water, filter, and purify with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 2:1 to obtain an intermediate product;

[0059] S3: 0.27 g of N-bromosuccinimide and 0.1 g of the intermediate product were dissolved in 10 mL of dichloromethane to obtain solution 1 and solution 2, and solution 1 was added dropwise to solution 2. The mixture was stirred for 24 h under light-proof conditions, and then evaporated in vacuo. The mixture was purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 1:2 to obtain a yellow-brown solid.

[0060] S4: The chopped carbon fiber was placed in a muffle furnace at 450°C for high temperature treatment for 3 hours, then taken out and soaked in a 0.1 mol / L sodium hydroxide solution for 3 hours, and dried at 60°C for 12 hours to obtain pretreated chopped carbon fiber. 0.4 g of yellowish brown solid was added to 5 mL of dichloromethane and stirred to obtain solution 3. Then 3 g of pretreated chopped carbon fiber was added to solution 3, heated and stirred at 70°C for 3 hours, filtered and dried to obtain the absorbing layer material.

[0061] This embodiment discloses a method for processing a multi-spectrum composite profiling camouflage material, comprising the following steps:

[0062] Step 1: 10 mL of distilled water, 2 g of nano titanium dioxide, 1 g of silicon dioxide, 0.1 g of dispersant, 0.01 g of defoamer and 0.3 g of binder are mixed and stirred to obtain an infrared reflection layer material, 8 g of epoxy resin and 1 g of aluminum powder are mixed and stirred to obtain a transition layer material, and 3 g of camouflage pigment and 12 g of nylon are mixed to obtain a camouflage layer material;

[0063] Step 2: Evenly apply the infrared reflective layer material on the surface of the PU hydrophobic base layer material, then evenly apply the transition layer material on the surface of the infrared reflective layer, then evenly cover the absorbing layer material on the surface of the transition layer, and finally, fix the camouflage layer material on the surface of the absorbing layer by glue. After drying, a multi-spectrum composite contoured camouflage layer material is obtained.

[0064] Embodiment 4: This embodiment discloses a method for preparing a PU hydrophobic matrix layer material, comprising the following steps:

[0065] Q1: 3.67 g of dichloromethylvinylsilane and 10.86 g of trimethylmonochlorosilane were added to a container, mixed and stirred for 15 min in an ice-water bath, and then 9.36 g of isopropanol was slowly added, and the reaction was continued for 45 min. After the reaction was completed, 4.21 mL of deionized water was added dropwise and the reaction was continued for 2 h. Then, stirring was stopped, and the mixture was allowed to stand for 10 min. The organic layer was washed, molecular sieves were added, filtered, and distilled under reduced pressure to obtain a colorless transparent liquid.

[0066] Q2: 3.72g of colorless transparent liquid and 1.52g of thioglycolic acid were added to a container, followed by 7.5mL of tetrahydrofuran, stirred and mixed for 60min, then 0.11g of benzoin diethyl ether was added, and the reaction was carried out under 365nm ultraviolet irradiation for 30min, then 0.8g of perfluorooctylethanol was added to 7mL of dichloromethane, stirred and added dropwise to the container, and the reaction was carried out for 36h, rotary evaporation, washing, and vacuum drying at 70℃ for 48h to obtain a hydrophobic organic matter;

[0067] Q3: 2kg of PU stone was ultrasonically cleaned in acetone and deionized water for 4 hours respectively, and then dried. Then 150g of hydrophobic organic matter was added to 1L of distilled water and ultrasonically stirred for 45 minutes to obtain a mixed solution. Then the dried PU stone was added to the mixed solution and ultrasonically oscillated for 3 hours. Then the PU stone was taken out, washed with distilled water, and dried at 70°C for 5 hours to obtain the PU hydrophobic matrix layer material.

[0068] This embodiment discloses a method for preparing an absorbing layer material, comprising the following steps:

[0069] S1: Add 14.93g of m-bromoacetophenone and 10.1g of thiophene-2-carboxaldehyde to a container containing 375mL of methanol, add 22.5mL of 2.5mol / L potassium hydroxide solution at 0℃, stir at room temperature for 12h, cool, filter, wash with petroleum ether, and recrystallize to obtain a light yellow solid; add 8.41g of light yellow solid, 10.25g of diethylamine and 9.1g of nitromethane to a container containing 210mL of methanol, heat at 90℃ for 12h, cool to 1℃ after the reaction, add 2.5mol / L of hydrochloric acid to acidify to pH=2, extract with dichloromethane, combine the organic phases, dry with anhydrous sodium sulfate, concentrate under reduced pressure, and purify with a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 10:1 to obtain a brown oil;

[0070] S2: Add 1.68g of brown oil and 13.08g of ammonium acetate to a container containing 96mL of ethanol, and heat to reflux at 90℃ for 24h under argon protection. After reflux, cool to 0℃, wash with petroleum ether, and filter to obtain a black solid; add 1.21g of black solid to 13mL of dichloromethane, stir to dissolve, and add 3.25mL of N,N-diisopropylethylamine dropwise at 1℃ under argon protection. After stirring for 45min, add 7.37mL of boron trifluoride ether, warm to room temperature, and stir to react for 48h. After the reaction, add the mixture to cold water, filter, and purify with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 2:1 to obtain an intermediate product;

[0071] S3: 0.49 g of N-bromosuccinimide and 0.18 g of the intermediate product were dissolved in 10 mL of dichloromethane to obtain solution 1 and solution 2, and solution 1 was added dropwise to solution 2. The mixture was stirred for 24 h under light-proof conditions, and then evaporated in vacuo. The mixture was purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 1:2 to obtain a yellow-brown solid.

[0072] S4: The chopped carbon fiber was placed in a muffle furnace at 450°C for high temperature treatment for 3 hours, then taken out and soaked in a 0.1 mol / L sodium hydroxide solution for 3 hours, and dried at 60°C for 12 hours to obtain pretreated chopped carbon fiber. 0.52 g of yellowish brown solid was added to 6.5 mL of dichloromethane and stirred to obtain solution 3. Then 3.8 g of pretreated chopped carbon fiber was added to solution 3, heated and stirred at 70°C for 3 hours, filtered and dried to obtain the absorbing layer material.

[0073] This embodiment discloses a method for processing a multi-spectrum composite profiling camouflage material, comprising the following steps:

[0074] Step 1: 12 mL of distilled water, 3 g of nano titanium dioxide, 2 g of silicon dioxide, 0.3 g of dispersant, 0.022 g of defoamer and 0.2 g of binder are mixed and stirred to obtain an infrared reflection layer material, 12 g of epoxy resin and 3 g of aluminum powder are mixed and stirred to obtain a transition layer material, and 6 g of camouflage pigment and 9 g of nylon are mixed to obtain a camouflage layer material;

[0075] Step 2: Evenly apply the infrared reflective layer material on the surface of the PU hydrophobic base layer material, then evenly apply the transition layer material on the surface of the infrared reflective layer, then evenly cover the absorbing layer material on the surface of the transition layer, and finally, fix the camouflage layer material on the surface of the absorbing layer by glue. After drying, a multi-spectrum composite contoured camouflage layer material is obtained.

[0076] Comparative Example 1: Compared with Example 2, in Comparative Example 1, during the preparation process of the PU hydrophobic base layer material, perfluorooctylethanol was not added, and other conditions remained unchanged.

[0077] Comparative Example 2: Compared with Example 2, in the preparation process of the absorbing layer material in Comparative Example 2, no thiophene-2-carboxaldehyde is added, and other conditions remain unchanged.

[0078] Comparative Example 3: Compared with Example 2, in the preparation process of the multi-spectrum composite contour camouflage layer material, ordinary PU material is used to replace the PU hydrophobic base layer material in Comparative Example 3, and other conditions remain unchanged.

[0079] Comparative Example 4: Compared with Example 2, in Comparative Example 4, in the preparation process of the multi-spectrum composite contour camouflage layer material, carbon fiber is used instead of the absorbing layer material, and other conditions remain unchanged.

[0080] Experimental example: The waterproof performance of the sample was tested according to GB / T 16777-2008, and the shielding performance of the sample was tested according to GJB 6190-2008. The test results are shown in Table 1:

[0081] Table 1

[0082]

[0083] It can be seen from the test results in Table 1 that the multi-spectrum composite profiling camouflage layer material prepared in Examples 2-4 of the present invention has excellent waterproof performance and shielding performance. By comparing Comparative Example 1 with Examples 2-4, it can be seen that the addition of perfluorooctylethanol can make the obtained multi-spectrum composite profiling camouflage layer material have excellent waterproof performance; by comparing Comparative Example 2 with Examples 2-4, it can be seen that the addition of thiophene-2-carboxaldehyde can make the obtained multi-spectrum composite profiling camouflage layer material have excellent shielding performance; by comparing Comparative Example 3 with Examples 2-4, it can be seen that the use of PU hydrophobic matrix layer material can make the obtained multi-spectrum composite profiling camouflage layer material have excellent waterproof performance; by comparing Comparative Example 4 with Examples 2-4, it can be seen that the use of absorbing layer material can make the obtained multi-spectrum composite profiling camouflage layer material have excellent shielding performance.

[0084] 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.

[0085] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. Multi-spectrum composite profiling camouflage material, characterized in that: The multi-spectrum composite profiling camouflage material comprises a PU hydrophobic matrix layer, an infrared reflection layer, a transition layer, an absorbing layer and a camouflage layer in sequence, wherein the PU hydrophobic matrix layer material is prepared from PU stone and hydrophobic organic matter; the infrared reflection layer material is prepared from distilled water, nano titanium dioxide, silicon dioxide, a dispersant, a defoaming agent and a binder; the transition layer material is prepared from epoxy resin and aluminum powder; the absorbing layer material is prepared from m-bromoacetophenone, thiophene-2-carboxaldehyde, nitromethane, ammonium acetate, N,N-diisopropylethylamine, N-bromosuccinimide and chopped carbon fiber; the camouflage layer material is composed of camouflage pigment and nylon; The method for preparing the wave absorbing layer material comprises the following steps: S1: Add m-bromoacetophenone and thiophene-2-carboxaldehyde to a container containing methanol, add potassium hydroxide solution under low temperature, stir at room temperature for reaction, cool, filter, wash, and recrystallize to obtain a light yellow solid; add the light yellow solid, diethylamine, and nitromethane to a container containing methanol, heat under reflux for reaction, cool, acidify, extract, combine the organic phases, dry, concentrate under reduced pressure, and purify to obtain a brown oil; S2: Add brown oil and ammonium acetate to a container containing ethanol, heat to reflux under argon protection, cool, wash, and filter to obtain a black solid after reflux. Add the black solid to dichloromethane, stir to dissolve, add N,N-diisopropylethylamine dropwise at low temperature under argon protection, continue stirring, add boron trifluoride etherate dropwise, heat, stir to react, add the mixture to cold water after the reaction is completed, filter, and purify to obtain an intermediate product. S3: N-bromosuccinimide and the intermediate product were dissolved in dichloromethane to obtain solution 1 and solution 2, solution 1 was added dropwise to solution 2, and the mixture was stirred to react in the dark, and vacuum evaporated and purified to obtain a yellow-brown solid; S4: placing the chopped carbon fiber in a muffle furnace for high-temperature treatment, then taking it out and soaking it in sodium hydroxide solution, drying it to obtain pretreated chopped carbon fiber, adding the yellowish brown solid into dichloromethane, stirring to obtain solution 3, and then adding the pretreated chopped carbon fiber into solution 3, heating and stirring, filtering, and drying to obtain the absorbing layer material.

2. The multi-spectrum composite profiling camouflage material according to claim 1, characterized in that: The preparation method of the PU hydrophobic matrix layer material comprises the following steps: Q1: Add dichloromethylvinylsilane and trimethylmonochlorosilane into a container, mix and stir in an ice-water bath, then slowly add isopropanol to continue the reaction. After the reaction is completed, add deionized water to continue the reaction, then stop stirring, let stand, wash the organic layer, add molecular sieves, filter, and distill under reduced pressure to obtain a colorless transparent liquid; Q2: Add a colorless transparent liquid and thioglycolic acid into a container, then add tetrahydrofuran, stir and mix evenly, add benzoin diethyl ether, irradiate with ultraviolet light for reaction, then add perfluorooctylethanol into dichloromethane, stir and add dropwise into the container, react, rotary evaporate, wash, and vacuum dry to obtain a hydrophobic organic substance; Q3: The PU stone is placed in acetone and deionized water for ultrasonic cleaning and then dried. The hydrophobic organic matter is then added to the distilled water and ultrasonically stirred to obtain a mixed solution. The dried PU stone is then added to the mixed solution and ultrasonically oscillated. The PU stone is then taken out, washed, and dried to obtain the PU hydrophobic matrix layer material.

3. The multi-spectrum composite profiling camouflage material according to claim 2, characterized in that: In Q1, the dosage ratio of dichloromethylvinylsilane, trimethyl monochlorosilane, isopropanol and deionized water is (2.82-3.67) g: (10.86-14.12) g: (7.2-9.36) g: (3.24-4.21) mL, the mixing time is 10-15 min, the reaction time is 30-45 min, the deionized water is added dropwise and the reaction time is 1-2 h, and the standing time is 10-20 min; in Q2, the colorless transparent liquid, thioglycolic acid, tetrahydrofuran, benzoin The dosage ratio of diethyl ether, perfluorooctylethanol and dichloromethane is (2.48-3.72) g: (1.01-1.52) g: (5-7.5) mL: (0.07-0.11) g: (0.53-0.8) g: (7-10.5) mL, the stirring mixing time is 45-60 min, the ultraviolet light wavelength of the ultraviolet irradiation reaction is 320-400 nm, the irradiation time is 15-30 min, the reaction time is 24-36 h, the vacuum drying temperature is 60-70 ° C, and the time is 36-48 h.

4. The multi-spectrum composite profiling camouflage material according to claim 2, characterized in that: In Q3, the ultrasonic cleaning time is 2-4 hours, the usage ratio of PU stone, hydrophobic organic matter and distilled water is (1-2) kg: (100-150) g: (1-2) L, the ultrasonic stirring time is 30-45 minutes, the ultrasonic oscillation time is 2-3 hours, washing is carried out with distilled water, the drying temperature is 60-70°C, and the time is 3-5 hours.

5. The multi-spectral composite profiling camouflage material according to claim 1, characterized in that: In the S1, the amount ratio of m-bromoacetophenone, thiophene-2-carboxaldehyde, methanol and potassium hydroxide solution is (9.95-14.93) g: (6.73-10.1) g: (250-375) mL: (15-22.5) mL, the low temperature environment temperature is 0-3 ° C, the concentration of potassium hydroxide solution is 2.5 mol / L, the stirring reaction time is 10-12 hours, and the washing is carried out with petroleum ether; the light yellow solid, diethylamine, nitromethane and methanol are The dosage ratio is (6.01-8.41) g: (7.32-10.25) g: (6.5-9.1) g: (150-210) mL, the heating reflux temperature is 80-90°C, the reaction time is 10-12h, cooled to 0-1°C, added with 2.5mol / L hydrochloric acid to acidify to pH=2, extracted with dichloromethane, dried with anhydrous sodium sulfate, and purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 10:

1.

6. The multi-spectrum composite profiling camouflage material according to claim 1, characterized in that: In the S2, the dosage ratio of the brown oil, ammonium acetate and ethanol is (1.4-1.68) g: (10.9-13.08) g: (80-96) mL, the heating reflux temperature is 90-95°C, the time is 20-24 h, the temperature is cooled to 0-1°C, and the product is washed with petroleum ether; the dosage ratio of the black solid, dichloromethane, N,N-diisopropylethylamine and boron trifluoride ether is (0.93-1.21) g: (10-13) mL: (2.5-3.25) mL: (5.67-7.37) mL, the low temperature environment temperature is 0-1°C, the stirring time is 30-45 min, the temperature is raised to room temperature, the stirring reaction time is 48-52 h, and the product is purified with a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 2:

1.

7. The multi-spectrum composite profiling camouflage material according to claim 1, characterized in that: In the S3, the dosage ratio of N-bromosuccinimide and the intermediate product is (0.27-0.49) g: (0.1-0.18) g, the stirring reaction time is 20-24 h, and the mixture is purified by a mixed solution of petroleum ether and ethyl acetate in a volume ratio of 1:2; in the S4, the high temperature treatment temperature is 400-450°C, the time is 2-3 h, the concentration of the sodium hydroxide solution is 0.1 mol / L, the soaking time is 2-3 h, the drying temperature is 60-70°C, the time is 10-12 h, the dosage ratio of the yellow-brown solid, dichloromethane and pretreated chopped carbon fiber is (0.4-0.52) g: (5-6.5) mL: (3-3.8) g, the heating and stirring temperature is 70-80°C, and the time is 2-3 h.

8. The method for processing a multi-spectrum composite profiling camouflage material according to any one of claims 1 to 7, characterized in that: The following steps are involved: Step 1: Mix and stir distilled water, nano titanium dioxide, silicon dioxide, dispersant, defoamer and binder to obtain infrared reflection layer material, mix and stir epoxy resin and aluminum powder to obtain transition layer material, and mix camouflage pigment and nylon to obtain camouflage layer material; Step 2: Evenly apply the infrared reflective layer material on the surface of the PU hydrophobic base layer material, then evenly apply the transition layer material on the surface of the infrared reflective layer, then evenly cover the absorbing layer material on the surface of the transition layer, and finally, fix the camouflage layer material on the surface of the absorbing layer by glue. After drying, a multi-spectrum composite contoured camouflage layer material is obtained.

9. The method for processing multi-spectrum composite profiling camouflage material according to claim 8, characterized in that: In the step 1, the dosage ratio of distilled water, nano titanium dioxide, silicon dioxide, dispersant, defoaming agent and binder is (10-12) mL: (2-3) g: (1-2) g: (0.1-0.3) g: (0.01-0.02) g: (0.2-0.3) g, the mass ratio of epoxy resin to aluminum powder is (8-12): (1-3), and the mass ratio of camouflage pigment to nylon is (3-6): (9-12).

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