CN110983797B - Thermal invisible flexible material and preparation method thereof - Google Patents
Thermal invisible flexible material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims description 59
- 229920002635 polyurethane Polymers 0.000 claims description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 229910002113 barium titanate Inorganic materials 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- -1 polydimethylsiloxane Polymers 0.000 claims description 13
- 229920003257 polycarbosilane Polymers 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 7
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 7
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 229920000555 poly(dimethylsilanediyl) polymer Polymers 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 59
- 229910018540 Si C Inorganic materials 0.000 description 12
- 238000002791 soaking Methods 0.000 description 5
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- 230000000052 comparative effect Effects 0.000 description 2
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- 238000001000 micrograph Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/142—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes mixture of polyurethanes with other resins in the same layer
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0006—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using woven fabrics
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
Abstract
The invention relates to a thermal invisible flexible material and a preparation method thereof. The method comprises the steps of taking dimethyl dichlorosilane, water-soluble carbon black solution, ethyl orthosilicate and the like as main raw materials, firstly preparing a SiC spinning solution precursor, spinning the SiC spinning solution precursor, and sintering at high temperature to prepare SiC ceramic fibers; spinning SiC ceramic fibers into fabrics; then infiltrating the SiC ceramic fiber fabric with carbon-silica sol, and sintering at high temperature to obtain the carbon-silica sol reinforced SiC ceramic fiber fabric; finally, coating BaTiO on the surface of the carbon-silica sol reinforced SiC ceramic fiber fabric3Polyurethane composite emulsion coating agent to prepare the thermal invisible flexible material. The far infrared emissivity of the thermal invisible flexible material prepared by the invention is only 0.32-0.38, and the material is very good in invisibility. The thermal invisible flexible material prepared by the invention has wide raw material source and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation of thermal invisible materials, and particularly relates to a thermal invisible flexible material and a preparation method thereof.
Background
The infrared detector can detect heat-generating objects to various degrees, and based on this principle, in order to realize the stealth of the heat-generating objects, the infrared detector must absorb or shield infrared rays. In modern war weapons, many weapons are expected to have stealth functionality, so that they may be left undiscovered and stealth is achieved.
At present, researches on heat stealth materials are reported, but the researches are few, Chinese invention patent application No. 200910308466.7 discloses a novel method for heat insulation of a spacecraft and heat stealth of an aircraft and a fourth substance form generating device, the method emits a special substance at the time and the position of the spacecraft which needs heat insulation protection or the aircraft prevents heat radiation from leaking, and the substance can be hidden by infrared detection to realize the heat stealth of the spacecraft; when the cooling device is applied, fluid or liquid substances are mainly sprayed in front of the heat radiation hidden part of the aircraft, and a flowing film with the functions of cooling and shielding is formed under the flushing of the head-on airflow; the heat-insulating material has the defect that the heat-insulating material is limited in use objects, namely the heat-insulating material is suitable for spacecrafts and is not necessarily suitable for objects with relatively low speed, such as automobiles or tanks.
With the increasing development of science and technology, the demand of the thermal invisible material is higher and higher. Literature research shows that the heat invisible materials with universality have fewer reports and are in need of further development and application.
Disclosure of Invention
The invention aims to provide a thermal invisible flexible material to solve the defects in the prior art, the thermal invisible flexible material is a special fabric, has a good thermal invisible function, and can be used as a shielding material for other heating objects after being wrapped by other heating objects.
The invention aims to provide a thermal invisible flexible material, which can be prepared by the following preparation method: taking dimethyl dichlorosilane, water-soluble carbon black solution, ethyl orthosilicate and the like as main raw materials, firstly preparing a SiC spinning solution precursor, spinning the SiC spinning solution precursor, and sintering at high temperature to prepare SiC ceramic fibers; spinning SiC ceramic fibers into fabrics; then soaking the SiC ceramic fiber fabric into carbon-silica sol, and sintering at high temperature to obtain the carbon-silica sol reinforced SiC ceramic fiberA fiber fabric; finally, coating BaTiO on the surface of the carbon-silica sol reinforced SiC ceramic fiber fabric3Polyurethane composite emulsion coating agent to prepare the thermal invisible flexible material.
The invention also aims to provide a preparation method of the thermal invisible flexible material, which comprises the following steps:
(1) preparing a SiC spinning solution precursor: under the atmosphere of helium, adding dimethyldichlorosilane and molten sodium into a toluene solvent, stirring for reaction at the temperature of 80-90 ℃ for 3-5 hours, standing for layering after the reaction is finished, and taking an upper-layer solution to obtain polydimethylsilane; adding polydimethylsiloxane into a high-pressure reaction kettle, heating to 400-500 ℃, setting the pressure to be 12-16 MPa, and reacting for 10-12 hours to obtain polycarbosilane; dissolving polycarbosilane in dimethylbenzene to prepare spinning solution.
Preferably, the mass to volume ratio of dimethyldichlorosilane (mL), molten sodium (g) and toluene solvent (mL) is: 1: 2-4: 10-20; the mass-volume ratio of polycarbosilane (g) to xylene (mL) in the spinning solution is as follows: 1: 10-20.
(2) Preparing the SiC ceramic fiber fabric: spinning the spinning solution prepared in the step (1) in a spinning system, and washing, oiling and drying the spun silk to obtain silk; sintering the silk thread for 8-12 hours at 1300-1500 ℃ in a nitrogen atmosphere to obtain SiC ceramic fiber; and preparing the SiC ceramic fiber fabric by the processes of unwinding, cabling, warping, drafting and weaving the SiC ceramic fiber.
Preferably, the temperature of the water washing is: 30-50 ℃; the oil bath temperature for oiling is 80-85 ℃; the drying temperature is 50-70 ℃.
Preferably, the weave structure of the SiC ceramic fiber fabric is as follows: 2/3 twill; the gram weight of the fabric is 300-400 g.m-2(ii) a The warp and weft density is: (15. + -.2). times. (15. + -.2)/root. cm-1。
(3) Preparing carbon-silanol sol: mixing deionized water and absolute ethyl alcohol to prepare a mixed solution a, dissolving water-soluble carbon black in the mixed solution a, stirring and reacting for 10-12 hours, and standing for 3-5 days to prepare carbon alcohol sol; mixing ethyl orthosilicate and absolute ethyl alcohol to prepare a mixed solution b, dropwise adding 1-5% diluted ammonia water into the mixed solution b, and stirring and dropwise adding for 1-3 hours to prepare silanol sol; the carbon-silicon sol is prepared by stirring and mixing the carbon-silicon sol and the silicon-silicon sol in a certain proportion.
Preferably, the volume ratio of the deionized water (mL) to the absolute ethyl alcohol (mL) in the mixed solution a is: 1: 2-4, wherein the mass-volume ratio of the water-soluble carbon black (g) to the mixed solution a (mL) is as follows: 1: 5-10; the volume ratio of the ethyl orthosilicate (mL) to the absolute ethyl alcohol (mL) in the mixed solution b is as follows: 1: 5-9; the volume ratio of the carbon alcohol sol (mL) to the silanol sol (mL) is as follows: 1: 1-3.
(4) Preparing a carbon-silica sol reinforced SiC ceramic fiber fabric: and (3) soaking the SiC ceramic fiber fabric prepared in the step (2) in the carbon-silanol sol prepared in the step (3), and sintering the soaked SiC ceramic fiber fabric for 3-5 hours at 1300-1500 ℃ in a nitrogen atmosphere to obtain the carbon-silica sol reinforced Si-C ceramic fiber fabric.
(5) Preparation of polyurethane emulsion coating agent: adding a proper amount of polyethylene glycol into a three-neck flask, and vacuumizing for 1-2 hours at the temperature of 90-95 ℃ to remove water; cooling to 60-80 ℃, adding toluene diisocyanate for reaction, wherein the reaction time is 1-2 h; determining the content of NCO by referring to an HG/T2409-1992 method, and adding dimethylolpropionic acid to carry out chain extension reaction for 0.5-1 h; cooling to 0-8 ℃, adding a mixed solution of isopropanol dissolved with sodium bisulfite and deionized water, and stirring at a high speed for 0.5-1 h; and after the reaction is finished, adjusting the pH value to 6-7 to obtain the waterborne polyurethane emulsion coating agent.
Preferably, the molecular weight of the polyethylene glycol is 500, and the mass molar ratio of the polyethylene glycol (mol), the toluene diisocyanate (mol) and the dimethylolpropionic acid (mol) is as follows: 1: 1-3: 0.2-0.4; the volume ratio of the isopropanol (mL) to the deionized water (mL) is 1: 2-4, and the mass ratio of the sodium bisulfite to the mixed solution is 1-5%.
(6)BaTiO3Preparing sol: mixing tetrabutyl titanate and Ba (OC)2H5)2Dissolving in anhydrous ethyl acetatePreparing mixed solution a by using alcohol, dissolving acetic acid in deionized water to prepare mixed solution b, dropwise adding the mixed solution b into the stirred mixed solution a for 3-5 hours to prepare BaTiO3And (3) sol.
Preferably, tetrabutyl titanate (mL), Ba (OC) in the mixed solution a2H5)2The volume ratio of (mL) to absolute ethyl alcohol (mL) is: 1: 1-3: 10-30, wherein the volume ratio of acetic acid (mL) to deionized water (mL) in the mixed solution b is as follows: 1: 10-20.
(7)BaTiO3Preparation of polyurethane composite emulsion coating agent: mixing the aqueous polyurethane emulsion prepared in the step (5) and the BaTiO prepared in the step (6)3Mixing the sol and stirring at high speed to obtain BaTiO3-polyurethane composite emulsion coating agents.
Preferably, the aqueous polyurethane emulsion prepared in the step (5) and the BaTiO prepared in the step (6)3The volume ratio of the sol is as follows: 1: 0.2-0.4.
(8) Preparing a thermal invisible flexible material: coating the carbon-silica sol reinforced Si-C ceramic fiber fabric prepared in the step (4) with BaTiO by adopting a dipping process3Baking the polyurethane composite emulsion coating agent at the temperature of 140-170 ℃ for 5-10 minutes to prepare BaTiO3The polyurethane composite emulsion coating agent is coated with carbon-silica sol reinforced Si-C ceramic fiber fabric, namely the thermal invisible flexible material.
The invention has the following remarkable advantages:
(1) the far infrared emissivity of the thermal invisible flexible material prepared by the invention is only 0.32-0.38, and the stealth is very good; even without coating with BaTiO3The far infrared emissivity of the polyurethane composite emulsion coating agent thermal stealth flexible material is also lower, and the polyurethane composite emulsion coating agent thermal stealth flexible material also has a better thermal stealth effect.
(2) The thermal invisible flexible material prepared by the invention selects SiC fibers with excellent wave absorbing performance as a main material, and in addition, the SiC ceramic fiber fabric is reinforced by adopting the carbon-silica sol, thereby being beneficial to the enhancement of the wave absorbing performance of the SiC fibers.
(3)BaTiO3And polyurethane have the performance of absorbing infrared rays, and BaTiO is used in the invention3Mixing into polyurethane emulsionTo prepare BaTiO3Polyurethane composite emulsion coating agents, achieving a better combination of the two.
Drawings
FIG. 1 is a schematic view of a spinning apparatus according to embodiments 1 to 3 of the present invention (1. nitrogen gas; 2. pressure vessel; 3. spinneret; 4. yarn; 5. traveling head; 6. drum; 7. temperature control device; 8. engine);
FIG. 2 is an electron microscope image of a SiC ceramic fiber fabric in example 1 of the present invention;
FIG. 3 is a schematic view of a coating apparatus according to embodiments 1 to 3 of the present invention (1. holder; 2. blade; 3. coating roll; 4. cooling and solidifying device; 5. drawing device; 6. winding device).
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this embodiment, a method for preparing a thermal invisible flexible material includes the following steps:
(1) preparing a SiC spinning solution precursor: under helium atmosphere, adding 10mL of dimethyldichlorosilane and 30g of molten sodium into 1500mL of toluene solvent, stirring for reaction at 85 ℃ for 4 hours, standing for layering after the reaction is finished, and taking the upper solution to obtain polydimethylsilane; adding polydimethylsiloxane into a high-pressure reaction kettle, heating to 450 ℃, setting the pressure to be 14MPa, and reacting for 11 hours to obtain polycarbosilane; the spinning dope was prepared by dissolving 100g of polycarbosilane in 1500mL of xylene.
(2) Preparing the SiC ceramic fiber fabric: enabling the spinning solution prepared in the step (1) to enter a spinning system for spinning, wherein the schematic diagram of spinning equipment is shown in figure 1, and the spun silk thread is subjected to water washing, oiling and drying treatment to prepare silk thread; sintering the silk thread at 1400 ℃ for 10 hours in a nitrogen atmosphere to obtain SiC ceramic fiber; preparing SiC ceramic fiber fabric by the processes of unwinding, cabling, warping, drafting and weaving, wherein an electron microscope image of the SiC ceramic fiber fabric is shown in figure 2; the temperature of the water washing is as follows: 40 ℃; the oil bath temperature for oiling is 83 ℃; the drying temperature is 60 ℃; the tissue structure of the SiC ceramic fiber fabric is as follows: 2/3 twill; fabric gramThe weight is 388.3 g.m-2(ii) a The warp and weft density is: (15. + -.2). times. (15. + -.2)/root. cm-1。
(3) Preparing carbon-silanol sol: mixing 100mL of deionized water and 300mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 10g of water-soluble carbon black in 75mL of the mixed solution a, stirring for reaction for 11 hours, and standing for 4 days to prepare carbon alcohol sol; mixing 20mL of ethyl orthosilicate and 140mL of absolute ethyl alcohol to prepare a mixed solution b, dropwise adding 3% diluted ammonia water into the mixed solution b, and stirring and dropwise adding for 2 hours to prepare silanol sol; stirring and mixing 100mL of carbon alcohol sol and 200mL of silicon alcohol sol to prepare the carbon-silicon sol.
(4) Preparing a carbon-silica sol reinforced SiC ceramic fiber fabric: and (3) soaking the SiC ceramic fiber fabric prepared in the step (2) in the carbon-silanol sol prepared in the step (3), and sintering the soaked SiC ceramic fiber fabric for 4 hours at 1400 ℃ in a nitrogen atmosphere to prepare the carbon-silica sol reinforced Si-C ceramic fiber fabric.
(5) Preparation of polyurethane emulsion coating: adding 0.1mol of polyethylene glycol with the molecular weight of 500 into a three-neck flask, and vacuumizing for 1.5h at 93 ℃ to remove water; cooling to 70 ℃, adding 0.2mol of toluene diisocyanate for reaction, wherein the reaction time is 1.5 h; determining the content of NCO by referring to an HG/T2409-1992 method, and adding 0.03mol of dimethylolpropionic acid to carry out chain extension reaction for 0.75 h; cooling to 4 ℃, adding a mixed solution of 20mL of isopropanol and 60mL of deionized water in which 3% sodium bisulfite is dissolved, and stirring at a high speed for 0.75 h; and after the reaction is finished, adjusting the pH value to 6.5 to obtain the aqueous polyurethane emulsion.
(6)BaTiO3Preparing sol: 10mL of tetrabutyl titanate and 20mL of Ba (OC)2H5)2Dissolving in 200mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 2mL of acetic acid in 30mL of deionized water to prepare a mixed solution b, and dropwise adding the mixed solution b into the stirred mixed solution a for 4 hours to prepare BaTiO3And (3) sol.
(7)BaTiO3Preparation of polyurethane composite emulsion coating agent: mixing 100mL of the aqueous polyurethane emulsion prepared in the step (5) with 30mL of BaTiO prepared in the step (6)3Mixing the sol and stirring at high speed to obtain BaTiO3-poly (A-co-poly (B-co-poly))A coating agent of polyurethane composite emulsion.
(8) Preparing a thermal invisible flexible material: dipping and coating BaTiO on the carbon-silica sol reinforced Si-C ceramic fiber fabric prepared in the step (4)3A polyurethane composite emulsion coating agent, a schematic drawing of a coating device is shown in figure 3, and the BaTiO is prepared by baking for 7 minutes at 150 DEG C3Coating carbon-silica sol reinforced Si-C ceramic fiber fabric with the polyurethane composite emulsion coating agent to obtain the thermal invisible flexible material a.
Example 2
In this embodiment, a method for preparing a thermal invisible flexible material includes the following steps:
(1) preparing a SiC spinning solution precursor: under the atmosphere of helium, adding 10mL of dimethyldichlorosilane and 20g of molten sodium into 1000mL of toluene solvent, stirring for reaction, keeping the reaction temperature at 80 ℃, keeping the reaction time for 3 hours, standing for layering after the reaction is finished, and taking the upper-layer solution to obtain polydimethylsilane; adding polydimethylsiloxane into a high-pressure reaction kettle, heating to 400 ℃, setting the pressure to be 12MPa, and reacting for 10 hours to obtain polycarbosilane; a spinning solution was prepared by dissolving 100g of polycarbosilane in 1000mL of xylene.
(2) Preparing the SiC ceramic fiber fabric: enabling the spinning solution prepared in the step (1) to enter a spinning system for spinning, wherein the schematic diagram of spinning equipment is shown in figure 1, and the spun silk thread is subjected to water washing, oiling and drying treatment to prepare silk thread; sintering the silk thread at 1300 ℃ for 8 hours under the nitrogen atmosphere to obtain SiC ceramic fiber; preparing SiC ceramic fiber fabric by the processes of unwinding, cabling, warping, drafting and weaving the SiC ceramic fiber; the temperature of the water washing is as follows: 30 ℃; the oil bath temperature for oiling is 81 ℃; the drying temperature is 50 ℃; the tissue structure of the SiC ceramic fiber fabric is as follows: 2/3 twill; the gram weight of the fabric is 359.2 g.m-2(ii) a The warp and weft density is: (15. + -.2). times. (15. + -.2)/root. cm-1。
(3) Preparing carbon-silanol sol: mixing 100mL of deionized water and 200mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 10g of water-soluble carbon black in 50mL of the mixed solution a, stirring for reaction for 10 hours, and standing for 3 days to prepare carbon alcohol sol; mixing 20mL of ethyl orthosilicate and 100mL of absolute ethyl alcohol to prepare a mixed solution b, dropwise adding 1% diluted ammonia water into the mixed solution b, and stirring and dropwise adding for 1 hour to prepare silanol sol; and stirring and mixing 100mL of carbon alcohol sol and 100mL of silicon alcohol sol to prepare the carbon-silicon sol.
(4) Preparing a carbon-silica sol reinforced SiC ceramic fiber fabric: and (3) soaking the SiC ceramic fiber fabric prepared in the step (2) in the carbon-silanol sol prepared in the step (3), and sintering the soaked SiC ceramic fiber fabric for 4 hours at 1400 ℃ in a nitrogen atmosphere to prepare the carbon-silica sol reinforced Si-C ceramic fiber fabric.
(5) Preparation of polyurethane emulsion coating: adding 0.1mol of polyethylene glycol with the molecular weight of 500 into a three-neck flask, and vacuumizing for 1.5h at 93 ℃ to remove water; cooling to 70 ℃, adding 0.1mol of toluene diisocyanate for reaction, wherein the reaction time is 1.5 h; determining the content of NCO by referring to an HG/T2409-1992 method, and adding 0.02mol of dimethylolpropionic acid to carry out chain extension reaction for 0.75 h; cooling to 0 ℃, adding a mixed solution of 20mL of isopropanol and 40mL of deionized water in which 1% sodium bisulfite is dissolved, and stirring at high speed for 0.75 h; and after the reaction is finished, adjusting the pH value to 6.5 to obtain the aqueous polyurethane emulsion.
(6)BaTiO3Preparing sol: 10mL of tetrabutyl titanate and 10mL of Ba (OC)2H5)2Dissolving in 100mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 2mL of acetic acid in 20mL of deionized water to prepare a mixed solution b, and dropwise adding the mixed solution b into the stirred mixed solution a for 4 hours to prepare BaTiO3And (3) sol.
(7)BaTiO3Preparation of polyurethane composite emulsion coating agent: mixing 100mL of the aqueous polyurethane emulsion prepared in the step (5) with 20mL of BaTiO prepared in the step (6)3Mixing the sol and stirring at high speed to obtain BaTiO3-polyurethane composite emulsion coating agents.
(8) Preparing a thermal invisible flexible material: dipping and coating BaTiO on the carbon-silica sol reinforced Si-C ceramic fiber fabric prepared in the step (4)3A polyurethane composite emulsion coating agent, a schematic drawing of a coating device is shown in figure 3, and the BaTiO is prepared by baking at 140 ℃ for 5 minutes3Carbon-silica sol reinforced Si-C ceramic coated with polyurethane composite emulsion coating agentAnd (3) the fiber fabric is the heat invisible flexible material b.
Example 3
In this embodiment, a method for preparing a thermal invisible flexible material includes the following steps:
(1) preparing a SiC spinning solution precursor: under helium atmosphere, adding 10mL of dimethyldichlorosilane and 40g of molten sodium into 2000mL of toluene solvent, stirring for reaction at 90 ℃ for 5 hours, standing for layering after the reaction is finished, and taking an upper layer solution to obtain polydimethylsilane; adding polydimethylsiloxane into a high-pressure reaction kettle, heating to 500 ℃, setting the pressure to be 16MPa, and reacting for 12 hours to obtain polycarbosilane; dissolving 100g of polycarbosilane in 2000mL of dimethylbenzene to prepare spinning solution;
(2) preparing the SiC ceramic fiber fabric: enabling the spinning solution prepared in the step (1) to enter a spinning system for spinning, wherein the schematic diagram of spinning equipment is shown in figure 1, and the spun silk thread is subjected to water washing, oiling and drying treatment to prepare silk thread; sintering the silk thread at 1500 ℃ for 12 hours in a nitrogen atmosphere to obtain SiC ceramic fiber; preparing SiC ceramic fiber fabric by the processes of unwinding, cabling, warping, drafting and weaving the SiC ceramic fiber; the temperature of the water washing is as follows: 40 ℃; the oil bath temperature for oiling is 85 ℃; the drying temperature is 70 ℃; the tissue structure of the SiC ceramic fiber fabric is as follows: 2/3 twill; the gram weight of the fabric is 396.8 g.m-2(ii) a The warp and weft density is: (15. + -.2). times. (15. + -.2)/root. cm-1。
(3) Preparing carbon-silanol sol: mixing 100mL of deionized water and 400mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 10g of water-soluble carbon black in 100mL of the mixed solution a, stirring for reaction for 12 hours, and standing for 5 days to prepare carbon alcohol sol; mixing 20mL of ethyl orthosilicate and 180mL of absolute ethyl alcohol to prepare a mixed solution b, dropwise adding 5% diluted ammonia water into the mixed solution b, and stirring and dropwise adding for 3 hours to prepare silanol sol; stirring and mixing 100mL of carbon alcohol sol and 300mL of silicon alcohol sol to prepare the carbon-silicon sol.
(4) Preparing a carbon-silica sol reinforced SiC ceramic fiber fabric: and (3) soaking the SiC ceramic fiber fabric prepared in the step (2) in the carbon-silanol sol prepared in the step (3), and sintering the soaked SiC ceramic fiber fabric for 4 hours at 1400 ℃ in a nitrogen atmosphere to prepare the carbon-silica sol reinforced Si-C ceramic fiber fabric.
(5) Preparation of polyurethane emulsion coating: adding 0.1mol of polyethylene glycol with the molecular weight of 500 into a three-neck flask, and vacuumizing for 1.5h at 93 ℃ to remove water; cooling to 70 ℃, adding 0.3mol of toluene diisocyanate for reaction, wherein the reaction time is 1.5 h; determining the content of NCO by referring to an HG/T2409-1992 method, and adding 0.04mol of dimethylolpropionic acid to carry out chain extension reaction for 0.75 h; cooling to 8 ℃, adding a mixed solution of 20mL of isopropanol and 80mL of deionized water in which 5% sodium bisulfite is dissolved, and stirring at a high speed for 1 h; and after the reaction is finished, adjusting the pH value to 6.5 to obtain the aqueous polyurethane emulsion.
(6)BaTiO3Preparing sol: 10mL of tetrabutyl titanate and 30mL of Ba (OC)2H5)2Dissolving the mixed solution in 300mL of absolute ethyl alcohol to prepare a mixed solution a, dissolving 2mL of acetic acid in 40mL of deionized water to prepare a mixed solution b, and dropwise adding the mixed solution b into the stirred mixed solution a for 5 hours to prepare BaTiO3And (3) sol.
(7)BaTiO3Preparation of polyurethane composite emulsion coating agent: mixing 100mL of the aqueous polyurethane emulsion prepared in the step (5) with 40mL of BaTiO prepared in the step (6)3Mixing the sol and stirring at high speed to obtain BaTiO3-polyurethane composite emulsion coating agents.
(8) Preparing a thermal invisible flexible material: dipping and coating BaTiO on the carbon-silica sol reinforced Si-C ceramic fiber fabric prepared in the step (4)3A polyurethane composite emulsion coating agent, a schematic drawing of a coating device is shown in figure 3, and the BaTiO is prepared by baking at 170 ℃ for 10 minutes3Coating carbon-silica sol reinforced Si-C ceramic fiber fabric with the polyurethane composite emulsion coating agent to obtain the thermal invisible flexible material C.
Comparative example 4
This example is a comparative example, and the thermal invisible flexible material in this example is not coated with the BaTiO 3-polyurethane composite emulsion coating agent. In this example, the preparation method is exactly the same as the steps (1), (2), (3) and (4) of example 3, and the thermal invisible flexible material d is prepared.
Application performance evaluation example:
the thermal invisible flexible materials a, b, c and d prepared in the specific embodiments 1-4 of the invention are tested for far infrared emissivity performance, the test method refers to the detection and evaluation of the far infrared performance of GB/T30127-2013 textiles, the far infrared emissivity is calculated, no less than 10 test samples are tested, and the test average value is taken. The test results are shown in the following table:
the lower the far infrared emissivity is, the better the stealth effect is. As can be seen from the table, the far infrared emissivity of the thermal invisible flexible materials a, b and c prepared by the invention is only 0.32-0.38, and the stealth is very good; even if the far infrared emissivity of the thermal invisible flexible material d which is not coated with the BaTiO 3-polyurethane composite emulsion coating agent is lower, the thermal invisible flexible material d also has a better invisible effect.
Claims (10)
1. The preparation method of the thermal invisible flexible material is characterized by comprising the following steps:
(1)BaTiO3preparation of polyurethane composite emulsion coating agent: mixing the aqueous polyurethane emulsion with BaTiO3Mixing the sol and stirring at high speed to obtain BaTiO3-a polyurethane composite emulsion coating agent;
(2) preparing a thermal invisible flexible material: coating BaTiO on the carbon-silica sol reinforced SiC ceramic fiber fabric by adopting a dipping process3Baking the polyurethane composite emulsion coating agent at the temperature of 140-170 ℃ for 5-10 minutes to prepare BaTiO3The polyurethane composite emulsion coating agent is coated with carbon-silica sol reinforced SiC ceramic fiber fabric, namely the thermal invisible flexible material.
2. The method for preparing the thermal invisible flexible material as claimed in claim 1, wherein the method for preparing the aqueous polyurethane emulsion in the step (1) comprises the following steps: adding polyethylene glycol into a three-neck flask, and vacuumizing for 1-2 hours at 90-95 ℃ to remove water; cooling to 60-80 ℃, adding toluene diisocyanate for reaction, wherein the reaction time is 1-2 h; determining the content of NCO by referring to an HG/T2409-1992 method, and adding dimethylolpropionic acid to carry out chain extension reaction for 0.5-1 h; cooling to 0-8 ℃, adding a mixed solution of isopropanol dissolved with sodium bisulfite and deionized water, and stirring at a high speed for 0.5-1 h; after the reaction is finished, adjusting the pH value to 6-7 to obtain a water-based polyurethane emulsion; the molecular weight of the polyethylene glycol is 500, and the mass molar ratio of the polyethylene glycol to the toluene diisocyanate to the dimethylolpropionic acid is as follows: 1mol, (1-3) mol, (0.2-0.4) mol; the volume ratio of the isopropanol to the deionized water is 1mL to (2-4) mL, and the mass ratio of the sodium bisulfite to the mixed solution is 1-5%.
3. The method for preparing a thermal invisible flexible material according to claim 1, wherein BaTiO in the step (1)3The preparation method of the sol comprises the following steps: mixing tetrabutyl titanate and Ba (OC)2H5)2Dissolving the mixed solution in absolute ethyl alcohol to prepare a mixed solution a, dissolving acetic acid in deionized water to prepare a mixed solution b, and dropwise adding the mixed solution b to the stirred mixed solution a for 3-5 hours to prepare BaTiO3Sol; tetrabutyl titanate and Ba (OC) in the mixed solution a2H5)2The volume ratio of the ethanol to the absolute ethyl alcohol is as follows: 1mL to (1-3) mL to (10-30) mL, wherein the volume ratio of acetic acid to deionized water in the mixed solution b is as follows: 1mL to (10-20) mL.
4. The method for preparing the thermal invisible flexible material according to claim 1, wherein the method for preparing the carbon-silica sol reinforced SiC ceramic fiber fabric in the step (2) comprises the following steps: and infiltrating the SiC ceramic fiber fabric into carbon-silica sol, and sintering the infiltrated SiC ceramic fiber fabric for 3-5 hours at 1300-1500 ℃ in a nitrogen atmosphere to obtain the carbon-silica sol reinforced SiC ceramic fiber fabric.
5. The method for preparing the thermal invisible flexible material as claimed in claim 4, wherein the method for preparing the carbon-silica sol comprises the following steps: mixing deionized water and absolute ethyl alcohol to prepare a mixed solution a, dissolving water-soluble carbon black in the mixed solution a, stirring and reacting for 10-12 hours, and standing for 3-5 days to prepare carbon alcohol sol; mixing ethyl orthosilicate and absolute ethyl alcohol to prepare a mixed solution b, dropwise adding 1-5% diluted ammonia water into the mixed solution b, and stirring and dropwise adding for 1-3 hours to prepare silanol sol; stirring and mixing the carbon alcohol sol and the silicon alcohol sol in a certain ratio to prepare carbon-silicon sol; the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution a is as follows: 1mL to (2-4) mL, wherein the mass-volume ratio of the water-soluble carbon black to the mixed solution a is as follows: 1g to (5-10) mL; the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol in the mixed solution b is as follows: 1mL to (5-9) mL; the volume ratio of the carbon alcohol sol to the silicon alcohol sol is as follows: 1mL to (1-3) mL.
6. The method for preparing the thermal invisible flexible material as claimed in claim 4, wherein the method for preparing the SiC ceramic fiber fabric comprises the following steps: spinning the spinning solution in a spinning system, and washing, oiling and drying the spun silk to obtain silk; sintering the silk thread for 8-12 hours at 1300-1500 ℃ in a nitrogen atmosphere to obtain SiC ceramic fiber; preparing SiC ceramic fiber fabric by the processes of unwinding, cabling, warping, drafting and weaving the SiC ceramic fiber; the temperature of the water washing is as follows: 30-50 ℃; the oil bath temperature for oiling is 80-85 ℃; the drying temperature is 50-70 ℃; the tissue structure of the SiC ceramic fiber fabric is as follows: 2/3 twill with a fabric weight of 300-400 g.m-2The warp and weft density is: (15. + -.2). times. (15. + -.2)/root. cm-1。
7. The method for preparing the heat invisible flexible material as claimed in claim 6, wherein the preparation method of the spinning solution comprises the following steps: under the atmosphere of helium, adding dimethyldichlorosilane and molten sodium into a toluene solvent, stirring for reaction at the temperature of 80-90 ℃ for 3-5 hours, standing for layering after the reaction is finished, and taking an upper-layer solution to obtain polydimethylsilane; adding polydimethylsiloxane into a high-pressure reaction kettle, heating to 400-500 ℃, setting the pressure to be 12-16 MPa, and reacting for 10-12 hours to obtain polycarbosilane; dissolving polycarbosilane in dimethylbenzene to prepare spinning solution.
8. The method for preparing the thermal invisible flexible material as claimed in claim 7, wherein the mass-to-volume ratio of the dimethyldichlorosilane to the molten sodium to the toluene solvent is as follows: 1mL, 2-4 g, 10-20 mL; the mass volume ratio of polycarbosilane to xylene in the spinning solution is as follows: 1g to (10-20) mL.
9. The method for preparing the thermal invisible flexible material as claimed in claim 1, wherein the aqueous polyurethane emulsion and BaTiO in the step (1)3The volume ratio of the sol is as follows: 1: 0.2-0.4.
10. A thermal invisible flexible material, which is prepared by the preparation method of the thermal invisible flexible material as claimed in any one of claims 1-9.
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