CN110578195B - Preparation method of wave-absorbing radiation-proof composite textile material - Google Patents
Preparation method of wave-absorbing radiation-proof composite textile material Download PDFInfo
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- CN110578195B CN110578195B CN201910704787.2A CN201910704787A CN110578195B CN 110578195 B CN110578195 B CN 110578195B CN 201910704787 A CN201910704787 A CN 201910704787A CN 110578195 B CN110578195 B CN 110578195B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2101/00—Inorganic fibres
- D10B2101/10—Inorganic fibres based on non-oxides other than metals
- D10B2101/12—Carbon; Pitch
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2101/00—Inorganic fibres
- D10B2101/10—Inorganic fibres based on non-oxides other than metals
- D10B2101/14—Carbides; Nitrides; Silicides; Borides
- D10B2101/16—Silicon carbide
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2101/00—Inorganic fibres
- D10B2101/20—Metallic fibres
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/01—Natural vegetable fibres
- D10B2201/02—Cotton
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- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Mechanical Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a preparation method of a wave-absorbing radiation-proof composite textile material, belonging to the technical field of textile materials. The invention prepares the radiation-proof composite textile material by adding the polyacrylonitrile-based carbon fiber and the silicon carbide fiber, the polyacrylonitrile-based carbon fiber and the silicon carbide fiber both belong to structural wave-absorbing materials, a structural member bearing compression, bending and shearing loads is prepared, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber form a circuit simulation structure in an orthogonal manner, the silicon carbide fiber and the carbon fiber which are arranged in the orthogonal manner form a plane conductive network, under the action of incident electromagnetic wave, induced current is generated, the electromagnetic wave energy is converted into heat energy through ohmic loss and eddy current loss and is lost, the attenuation of electromagnetic waves is enhanced, in addition, the wave absorbing screen formed by the silicon carbide fibers which are arranged in an orthogonal mode can play a role of a reflecting screen, the electromagnetic waves reflected from the surface of the wave absorbing screen and the electromagnetic waves reflected from the polycrystalline iron fiber reflecting layer can generate a phase cancellation effect, and the radiation protection capability of the wave absorbing screen is improved.
Description
Technical Field
The invention relates to a preparation method of a wave-absorbing radiation-proof composite textile material, belonging to the technical field of textile materials.
Background
The development of electronic technology has driven the prosperity of the electronic industry, small as electric shavers, mobile phones, tablets, computers, televisions and the like, large as mobile phone signal towers, high-voltage transmission lines, satellite communication, remote sensing, radar and the like, and the daily life of people is closely related to electronic equipment. However, electronic products and large electronic devices generate a large amount of electromagnetic radiation with different wavelengths, and the electromagnetic radiation is flooded around people to cause electromagnetic pollution, so that work and bodies of people are damaged to a certain extent. The hazards of electromagnetic contamination are primarily manifested in two ways.
1. Interfering with normal operation of the instrument: the wide distribution of electromagnetic waves invisibly disturbs the normal operation of various instruments. Electronic and electrical equipment and other equipment can break down due to electromagnetic wave interference, so that various precise instruments are greatly lost economically, and are difficult to accurately operate due to the electromagnetic wave interference, transmission of command signals is influenced, and secondary damage is caused; electromagnetic waves interfere with the precise positioning of military weapons, directly damaging the military forces of attack in war.
2. Harming the health: the harm of electromagnetic radiation to the human body is mainly classified into three types: thermal effects, non-thermal effects, cumulative effects (carcinogenic, mutagenic, and teratogenic).
(1) Thermal effect: the phenomenon that the body of a human body is heated up due to electromagnetic radiation is a heat effect. Caused by the rise of the body temperature
Various uncomfortable symptoms, including visual deterioration, memory deterioration, dizziness, headache, insomnia, neurasthenia, accelerated heartbeat, bradycardia, arrhythmia, leukopenia, immunologic function reduction and the like, can cause fatal damage such as myocardial infarction when serious. The temperature of each organ in the body is excessively increased, so that the organ is easily damaged irreversibly.
(2) Non-thermal effect: the weak electromagnetic field of human organs and tissues is affected by electromagnetic radiation as a non-thermal effect. Mainly includes the decline of the function of the nervous system, such as bradycardia; decreased sensory system, such as decreased olfactory function; low immune system capacity; endocrine disorders.
(3) Cumulative effect: the human body is damaged by electromagnetic radiation again before being repaired after the heating effect and the non-heating effect, and the damage to the human body is accumulated, which is an accumulation effect. The cumulative effect is a permanent and irreversible hazard to the human body. Therefore, there is a need for radiation protection, which has led to serious diseases even if the power and frequency of electromagnetic waves are low.
People pay attention to the harm caused by electromagnetic radiation, and the world health organization determines electromagnetic pollution as the fourth global pollution after atmospheric pollution, water pollution and noise pollution [8 ]. The protection mode aiming at the electromagnetic pollution is mainly two, one is to realize the protection of a target object by increasing reflection through high impedance on the surface; the other is to achieve protection by attenuation of electromagnetic waves through absorption of materials, wherein the mode of achieving protection by increasing reflection, namely electromagnetic shielding, is the main protection method.
The development of the wave-absorbing material is from the traditional wave-absorbing material such as graphite, ferrite, silicon carbide, barium titanate and the like to the novel wave-absorbing material such as intelligent stealth material, metamaterial, nano wave-absorbing material and the like [ |4], and the wave-absorbing material is developed in the direction of thin thickness, light weight, wide frequency band and strong absorption from the single mode mainly based on coating to the current situation of coexistence of multiple modes, and can even meet the requirements of some special purposes, such as high temperature resistance, strong environmental adaptability, radiation resistance and the like, and is widely applied to military fields such as warplanes, cruise missiles, naval vessels and the like. The important role of the wave-absorbing material in social life and national defense construction is not negligible, and higher requirements are provided for developing the wave-absorbing material.
The wave-absorbing material is a functional material which can effectively absorb incident electromagnetic waves, convert electromagnetic energy into heat energy and consume or enable the interference of the electromagnetic waves to be cancelled, and therefore the echo intensity of a target is obviously weakened. The absorbing material has very important application value in both military and civil fields. The wave-absorbing material is applied to the radar and the radio communication system, so that the interference between communication lines can be effectively avoided, and the sensitivity of the radar and the communication equipment is improved, thereby improving the communication quality; the use of high frequency communication systems and microwave heating devices also requires the use of absorbing materials to prevent electromagnetic radiation and leakage, thereby protecting the health and safety of the operator.
The electromagnetic wave pollution can seriously harm human health, in particular to people with weak physical quality, such as pregnant women and the like. In addition, electromagnetic waves can cause serious damage to the normal operation of communication equipment and electrical and electronic equipment. In the military field and the communication field, leakage of electromagnetic waves can also cause secret leakage. Therefore, the development of various electromagnetic wave protective materials is always a research hotspot and also a market hotspot. In particular to a textile fabric with the function of preventing electromagnetic wave radiation, which has great market demand. Because in daily life, with the increasing popularization of various electronic devices, people can contact a large amount of electromagnetic waves every day, and researches have shown that the existence of strong electromagnetic waves is harmful to the health of human bodies, especially to special people, such as pregnant women, old people, workers in special industries and the like.
In real life, electromagnetic waves of various frequency bands coexist, and therefore, it is desired to develop a material having a good electromagnetic wave absorption capability in an ultra-wide frequency range, both by researchers and in the market. It is known that in order to provide a textile fabric with electromagnetic radiation protection, various media capable of absorbing or reflecting electromagnetic waves must be added to the textile fabric. However, the absorption or reflection capability of a general medium to electromagnetic waves is closely related to its components or morphology structure, so if a textile fabric has good electromagnetic wave protection capability under a very wide frequency, multiple types of electromagnetic wave absorption or reflection media are often required to be added, and if a large amount of media are added, two technical problems are faced:
1. how to load a large amount of media into the textile fabric. There are two general methods for loading media into textile fabrics: firstly, coating the surface of the textile fabric; secondly, the medium is adhered to the fabric through some adhesives. It is clear that in both methods it is extremely difficult to load a large amount of media into the fabric.
2. Too much medium is loaded on the fabric to inevitably cause the reduction of the textile performance of the fabric. The textile fabric is finally required to be made into various wearing articles, so that certain textile performance requirements such as flowability, bendability, toughness and the like are met. Too much loading medium inevitably affects the textile performance, thus being not beneficial to the large-scale application of products.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that in the prior art, a large amount of medium is very difficult to load into the fabric, and the textile performance of the fabric is inevitably reduced due to too much medium being loaded onto the fabric, the preparation method of the wave-absorbing radiation-proof composite textile material is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) placing the cotton fibers in an opener, and pre-opening for 10-20 min at normal temperature to obtain pre-opened cotton fibers;
(2) adding polycrystalline iron fibers, silicon carbide fibers and polyacrylonitrile-based carbon fibers into pre-opened cotton fibers, placing the cotton fibers in a wool blending machine, and blending for 20-30 min at normal temperature to obtain mixed fibers;
(3) opening and picking the mixed fibers, then drawing the mixed fibers at the rotating speed of a front roller of 700-750 r/min after a cotton carding process to obtain the blended fibers;
(4) putting the fibers which are added in the spinning process into a roving machine, and performing roving at the rotating speed of a front roller of 200-300 r/min for 20-40 min to obtain a roving yarn;
(5) putting the rough spun yarn into a fine spinning machine, and fine spinning at the spun yarn spindle speed of 6000-6200 r/min for 30-40 min to obtain fine spun yarn;
(6) and (3) placing the fine spun yarns in an automatic winder, and performing a winding process for 1-2 hours at the rotating speed of 850-900 r/min at normal temperature to obtain the radiation-proof composite textile material.
The weight parts of the cotton fiber, the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber are 80-100 parts of the cotton fiber, 20-25 parts of the polycrystalline iron fiber, 8-10 parts of the silicon carbide fiber and 8-10 parts of the polyacrylonitrile-based carbon fiber.
The opening and picking process in the step (3) is carried out under the conditions of the ration of 300-400 g/m and the fixed length of 20-30 m.
The conditions of the roving in the step (4) are that the roller gauge is 22mm multiplied by 35mm, the drafting multiple of the back zone is 1, the relative humidity is 80 percent and the temperature is 25 ℃.
The fine spinning condition of the step (5) is that the twist is 50 twist/10 cm, the relative humidity is 75 percent, and the temperature is 25 ℃.
The specific preparation steps of the polycrystalline iron fiber in the step (2) are as follows:
(1) adding a sodium hydroxide solution into a ferrous sulfate solution at a flow rate of 5-10 mL/min, stirring and reacting for 10-15 min at a rotation speed of 160-200 r/min under a water bath condition of 15-20 ℃, dropwise adding sulfuric acid with a mass concentration of 1% to adjust the pH to 4-5, and obtaining a ferrous hydroxide colloid;
(2) introducing air into the ferrous hydroxide colloid at a flow rate of 10-20 mL/min for 3-5 min for oxidation reaction to obtain an oxidation reactant;
(3) adding the oxidation reactant into deionized water, and stirring at the rotating speed of 200-240 r/min for 10-20 min at normal temperature to obtain a mixed solution;
(4) adding a sodium silicate solution into the mixed solution, stirring at the normal temperature at the rotating speed of 240-280 r/min for 30-40 min, introducing carbon dioxide gas at the air flow speed of 20-30 mL/mim to adjust the pH value to 5.8-6.2, filtering out liquid, washing, and drying to obtain silicon-coated iron fibers;
(5) dehydrating the silicon-coated iron fiber for 4-6 hours at the temperature of 200-400 ℃ to obtain a dehydrated product;
(6) and (3) placing the dehydrated product into a quartz vessel, placing the quartz vessel into a reduction furnace, introducing nitrogen-hydrogen mixed gas, calcining for 4-6 hours at the temperature of 400-600 ℃, and cooling to room temperature along with the furnace to obtain the polycrystalline iron fiber.
The weight parts of the ferrous sulfate solution, the sodium hydroxide solution, the sodium silicate solution and 100-120 parts of deionized water are 50-60 parts of 25% ferrous sulfate solution, 10-12 parts of 5% sodium hydroxide solution, 20-30 parts of 10% sodium silicate solution and 100-120 parts of deionized water.
The volume ratio of the nitrogen to the hydrogen in the nitrogen-hydrogen mixed gas in the step (6) is 1:1, the gas is introduced at a speed of 120-140 mL/min.
The silicon carbide fiber prepared in the step (2) comprises the following specific preparation steps:
(1) placing polydimethylsiloxane into a reaction kettle, introducing high-purity nitrogen at the air flow rate of 40-60 mL/min for protection, heating to 200 ℃ at the heating rate of 5 ℃/min, preserving heat for 20-40 min, and cooling to normal temperature to obtain a polycarbosilane primary product;
(2) adding the polycarbosilane primary product into dimethylbenzene, and stirring at the normal temperature at the rotating speed of 300-400 r/min for 20-30 min to obtain a mixed solution;
(3) placing the mixed solution under the conditions of the pressure of 300-400 KPa and the temperature of 340-360 ℃ for 2-4 times of reduced pressure distillation, and cooling to room temperature to obtain polycarbosilane;
(4) putting polycarbosilane into a melt spinning machine, introducing nitrogen at the air flow rate of 40-50 mL/min for protection, extruding under the conditions of the pressure of 0.2-0.4 MPa and the temperature of 240-260 ℃, and cooling to room temperature to obtain polycarbosilane fiber precursor;
(5) placing the polycarbosilane fiber precursor in a vertical non-melting furnace, heating the polycarbosilane fiber precursor to 180 ℃ from normal temperature at the heating rate of 3-5 ℃/min, preserving the heat, performing non-melting treatment for 20-30 min, and cooling the polycarbosilane fiber precursor to room temperature along with the furnace to obtain non-melting polycarbosilane fiber;
(6) putting the fiber into a quartz boat, putting the quartz boat into a corundum tube, introducing nitrogen at the air flow rate of 40-60 mL/min for protection, heating the quartz boat to 1200 ℃ from the normal temperature at the heating rate of 5 ℃/min, carrying out heat preservation and calcination for 1-2 h, and cooling the quartz boat to the room temperature along with the tube to obtain the silicon carbide fiber with the average diameter of 0.12-0.16 mm.
The weight parts of the polydimethylsilane and the dimethylbenzene are 40-50 parts of the polydimethylsilane and 100-120 parts of the dimethylbenzene.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention takes the cotton fiber as the base material to prepare the radiation-proof composite textile material, the cotton fiber is an important raw material in the textile industry, the cotton fiber is a porous substance, and a large amount of hydrophilic groups exist on cellulose macromolecules, so the material has better hygroscopicity, is soft and warm-keeping, is slender and soft, has good flexibility and spinnability, can conveniently carry out various textile processing, takes the cotton fiber as the base material, and can improve the textile performance, the comfort and the air permeability of the material by well adsorbing and tangling other functional fibers together.
(2) The invention prepares the radiation-proof composite textile material by adding the polyacrylonitrile-based carbon fiber and the silicon carbide fiber, both the polyacrylonitrile-based carbon fiber and the silicon carbide fiber belong to structural wave-absorbing materials, which can not only absorb electromagnetic waves and reduce echo energy, but also can be made into structural members bearing compression, bending and shearing loads, compared with wave-absorbing coatings, the structural wave-absorbing materials do not have the problems of surface denudation, rough surface and extra weight increment, are not limited by thickness, are beneficial to widening absorption frequency bands, and do not influence the textile performance of base materials, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber form a circuit simulation structure in an orthogonal way, the silicon carbide fiber and the carbon fiber which are arranged in an orthogonal way form a plane conductive network, generate induced current under the action of incident electromagnetic waves, convert the electromagnetic wave energy into heat energy through ohmic loss and eddy current loss, the fiber spacing is reduced, the ohmic loss is increased, the attenuation of electromagnetic waves is enhanced, in addition, the wave absorbing screen formed by the silicon carbide fibers which are orthogonally arranged can play a role of a reflecting screen, the electromagnetic waves reflected from the surface of the wave absorbing screen and the electromagnetic waves reflected from a polycrystalline iron fiber reflecting layer can generate a phase cancellation effect, the radiation protection capability of the wave absorbing screen is improved, the monofilament diameter of the polyacrylonitrile-based carbon fiber is thin, the external surface area is large, a large number of holes are opened on the fiber surface, the polyacrylonitrile-based carbon fiber can be effectively adsorbed between the silicon carbide fibers and the cotton fibers, and the form of the polyacrylonitrile-based carbon fiber is various, so that the polyacrylonitrile-based carbon fiber can be freely processed into products with various forms such as cloth, felt;
(3) the invention prepares the radiation-proof composite textile material by adding the polycrystalline iron fiber, wherein the polycrystalline iron fiber is a functional material, the diameter of the polycrystalline iron fiber is between the micron and nanometer level, and the polycrystalline iron fiber is effective in the fiber length direction
The magnetic conductivity is very high, a good shielding effect on radiation can be achieved, the polycrystalline iron fibers and the cotton fibers are blended together to prepare the metal fiber fabric, a metal net is formed, a good radiation-proof effect can be achieved, and the prepared metal fiber fabric is stable in performance, washable, good in air permeability, attractive in style and good in textile performance.
Detailed Description
Weighing 40-50 parts of polydimethylsilane and 100-120 parts of dimethylbenzene respectively according to parts by weight, placing the polydimethylsilane in a reaction kettle, introducing high-purity nitrogen at an air flow rate of 40-60 mL/min for protection, heating to 200 ℃ at a heating rate of 5 ℃/min, preserving heat for 20-40 min, cooling to normal temperature to obtain a polycarbosilane primary product, adding the polycarbosilane primary product into the dimethylbenzene, stirring at a rotating speed of 300-400 r/min for 20-30 min at normal temperature to obtain a mixed solution, placing the mixed solution under the conditions of a pressure of 300-400 KPa and a temperature of 340-360 ℃ for reduced pressure distillation for 2-4, cooling to room temperature to obtain polycarbosilane, placing the polycarbosilane in a melt spinning machine, introducing nitrogen at an air flow rate of 40-50 mL/min for protection, extruding under the conditions of a pressure of 0.2-0.4 MPa and a temperature of 240-260 ℃, cooling to room temperature to obtain polycarbosilane protofilament, placing polycarbosilane fiber precursor in a vertical non-melting furnace, heating from normal temperature to 180 ℃ at the heating rate of 3-5 ℃/min, preserving heat, carrying out non-melting treatment for 20-30 min, cooling to room temperature along with the furnace to obtain non-melting polycarbosilane fiber, placing the fiber in a quartz boat, placing the quartz boat in a corundum tube, introducing nitrogen at the air flow rate of 40-60 mL/min for protection, heating from normal temperature to 1200 ℃ at the heating rate of 5 ℃/min, preserving heat, calcining for 1-2 h, and cooling to room temperature along with the tube to obtain silicon carbide fiber with the average diameter of 0.12-0.16 mm; respectively weighing 50-60 parts by weight of 25% ferrous sulfate solution, 10-12 parts by weight of 5% sodium hydroxide solution, 20-30 parts by weight of 10% sodium silicate solution and 100-120 parts by weight of deionized water, adding the sodium hydroxide solution into the ferrous sulfate solution at a flow rate of 5-10 mL/min, stirring and reacting for 10-15 min at a rotation speed of 160-200 r/min under a water bath condition of 15-20 ℃, dropwise adding 1% sulfuric acid to adjust the pH value to 4-5 to obtain a ferrous hydroxide colloid, introducing air into the ferrous hydroxide colloid at a flow rate of 10-20 mL/min for 3-5 min to perform an oxidation reaction to obtain an oxidation reactant, adding the oxidation reactant into the deionized water, stirring for 10-20 min at a rotation speed of 200-240 r/min at normal temperature to obtain a mixed solution, adding the sodium silicate solution into the mixed solution, stirring at the rotating speed of 240-280 r/min for 30-40 min at normal temperature, introducing carbon dioxide gas at the air flow speed of 20-30 mL/mm to adjust the pH value to 5.8-6.2, filtering out liquid, washing and drying to obtain silicon-coated iron fiber, dehydrating the silicon-coated iron fiber at the temperature of 200-400 ℃ for 4-6 h to obtain a dehydrated product, placing the dehydrated product into a quartz dish, placing the quartz dish in a reduction furnace, and introducing the mixture into the reduction furnace at the air flow speed of 120-140 mL/min in a volume ratio of 1: calcining the nitrogen-hydrogen mixed gas of 1 at 400-600 ℃ for 4-6 h, and cooling to room temperature along with the furnace to obtain polycrystalline iron fibers; respectively weighing 80-100 parts of cotton fiber, 20-25 parts of polycrystalline iron fiber, 8-10 parts of silicon carbide fiber and 8-10 parts of polyacrylonitrile-based carbon fiber according to parts by weight, placing the cotton fiber in an opener, pre-opening for 10-20 min at normal temperature to obtain pre-opened cotton fiber, adding the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber into the pre-opened cotton fiber, placing in a wool-spinning machine, wool-spinning for 20-30 min at normal temperature to obtain mixed fiber, opening and cleaning the mixed fiber at the conditions of the fixed quantity of 300-400 g/m and the fixed length of 20-30 m, drawing at the front roller rotating speed of 700-750 r/min after cotton carding process to obtain the blended fiber, placing the blended and post-added fiber in a roving machine, roving at the roller spacing of 22mm multiplied by 35mm, the drafting multiple of the rear area of 1, the relative humidity of 80%, and the temperature of 25 ℃ at the front roller rotating speed of 200-300 r/min, and (3) obtaining a coarse spun yarn, placing the coarse spun yarn in a fine spinning machine, performing fine spinning at the spinning spindle speed of 6000-6200 r/min for 30-40 min under the conditions of 50-10 cm twist for fixed twist, 75% relative humidity and 25 ℃ to obtain a fine spun yarn, placing the fine spun yarn in an automatic bobbin winder, and performing a bobbin winding process at the rotating speed of 850-900 r/min for 1-2 h at normal temperature to obtain the wave-absorbing and radiation-proof composite textile material.
Example 1
Respectively weighing 40 parts of polydimethylsilane and 100 parts of dimethylbenzene according to parts by weight, placing the polydimethylsilane in a reaction kettle, introducing high-purity nitrogen at the air flow rate of 40mL/min for protection, heating to 200 ℃ at the heating rate of 5 ℃/min, preserving heat for 20min, cooling to normal temperature to obtain a polycarbosilane primary product, adding the polycarbosilane primary product into the dimethylbenzene, stirring at the normal temperature at the rotating speed of 300r/min for 20min to obtain a mixed solution, placing the mixed solution under the conditions of the pressure of 300KPa and the temperature of 340 ℃ for reduced pressure distillation 2, cooling to room temperature to obtain polycarbosilane, placing the polycarbosilane in a melt spinning machine, introducing nitrogen at the air flow rate of 40mL/min for protection, extruding under the conditions of the pressure of 0.2MPa and the temperature of 240 ℃, cooling to the room temperature to obtain a polycarbosilane fiber precursor, placing the polycarbosilane fiber precursor in a vertical infusible furnace, heating to 180 ℃ from normal temperature at a heating rate of 3 ℃/min, preserving heat, carrying out non-melting treatment for 20min, cooling to room temperature along with the furnace to obtain non-melting polycarbosilane fiber, putting the fiber into a quartz boat, putting the quartz boat into a corundum tube, introducing nitrogen at an air flow rate of 40mL/min for protection, heating to 1200 ℃ from normal temperature at a heating rate of 5 ℃/min, preserving heat, calcining for 1h, and cooling to room temperature along with the tube to obtain silicon carbide fiber with the average diameter of 0.12 mm; respectively weighing 50 parts by weight of 25% ferrous sulfate solution with mass concentration, 10 parts by weight of 5% sodium hydroxide solution with mass concentration, 20 parts by weight of 10% sodium silicate solution and 100 parts by weight of deionized water, adding the sodium hydroxide solution into the ferrous sulfate solution at the flow rate of 5mL/min, stirring and reacting for 10min at the rotation speed of 160r/min under the condition of water bath at 15 ℃, dropwise adding 1% sulfuric acid with mass concentration to adjust the pH value to 4 to obtain a ferrous hydroxide colloid, introducing air into the ferrous hydroxide colloid at the flow rate of 10mL/min for 3min to perform oxidation reaction to obtain an oxidation reactant, adding the oxidation reactant into the deionized water, stirring for 10min at the rotation speed of 200r/min at normal temperature to obtain a mixed solution, adding the sodium silicate solution into the mixed solution, stirring for 30min at the rotation speed of 240r/min at normal temperature, introducing carbon dioxide gas at the air flow rate of 20mL/mim to adjust the pH value to 5.8, filtering out liquid, washing and drying to obtain silicon-coated iron fiber, dehydrating the silicon-coated iron fiber for 4 hours at the temperature of 200 ℃ to obtain a dehydrated product, putting the dehydrated product into a quartz dish, putting the quartz dish into a reduction furnace, and introducing the dehydrated product into the reduction furnace at the air flow rate of 120mL/min and the volume ratio of 1:1, calcining for 4 hours at 400 ℃, and cooling to room temperature along with the furnace to obtain polycrystalline iron fibers; respectively weighing 80 parts of cotton fiber, 20 parts of polycrystalline iron fiber, 8 parts of silicon carbide fiber and 8 parts of polyacrylonitrile-based carbon fiber according to parts by weight, placing the cotton fiber in an opener, pre-opening for 10min at normal temperature to obtain pre-opened cotton fiber, adding the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber into the pre-opened cotton fiber, placing the pre-opened cotton fiber in a wool-spinning machine, wool-spinning for 20min at normal temperature to obtain mixed fiber, opening and cleaning the mixed fiber at the conditions of a fixed quantity of 300g/m and a fixed length of 20m, carding, drawing at a front roller rotating speed of 700r/min to obtain blended fiber, placing the blended and post-added fiber in a roving machine, roving at a front roller rotating speed of 200r/min for 20min under the conditions of a roller gauge of 22mm multiplied by 35mm, a rear zone drafting multiple of 1, a relative humidity of 80% and a temperature of 25 ℃, and (3) obtaining a coarse spun yarn, placing the coarse spun yarn in a fine spinning machine, performing fine spinning at the speed of 6000r/min of a fine yarn spindle for 30min under the conditions of 50-twist-yarn length of 10cm, 75% relative humidity and 25 ℃ to obtain a fine spun yarn, placing the fine spun yarn in an automatic bobbin winder, and performing a bobbin winding process at the rotating speed of 850r/min for 1h at normal temperature to obtain the wave-absorbing radiation-proof composite textile material.
Example 2
Respectively weighing 45 parts of polydimethylsilane and 110 parts of dimethylbenzene according to parts by weight, placing the polydimethylsilane in a reaction kettle, introducing high-purity nitrogen at an air flow rate of 560mL/min for protection, heating to 200 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min, cooling to normal temperature to obtain a polycarbosilane primary product, adding the polycarbosilane primary product into the dimethylbenzene, stirring at a rotating speed of 350r/min for 25min at normal temperature to obtain a mixed solution, placing the mixed solution under the conditions of a pressure of 350KPa and a temperature of 350 ℃, carrying out reduced pressure distillation for 3, cooling to room temperature to obtain polycarbosilane, placing the polycarbosilane in a melt spinning machine, introducing nitrogen at an air flow rate of 45mL/min for protection, extruding under the conditions of a pressure of 0.3MPa and a temperature of 250 ℃, cooling to room temperature to obtain a polycarbosilane fiber precursor, placing the polycarbosilane fiber precursor in a vertical non-melting furnace, heating to 180 ℃ from normal temperature at a heating rate of 4 ℃/min, preserving heat, carrying out non-melting treatment for 25min, cooling to room temperature along with a furnace to obtain non-melting polycarbosilane fiber, putting the fiber into a quartz boat, putting the quartz boat into a corundum tube, introducing nitrogen at an air flow rate of 50mL/min for protection, heating to 1200 ℃ from normal temperature at a heating rate of 5 ℃/min, carrying out heat preservation and calcination for 1.5h, and cooling to room temperature along with the tube to obtain silicon carbide fiber with the average diameter of 0.14 mm; respectively weighing 55 parts by weight of 25% ferrous sulfate solution with mass concentration, 11 parts by weight of 5% sodium hydroxide solution with mass concentration, 25 parts by weight of 10% sodium silicate solution and 110 parts by weight of deionized water, adding the sodium hydroxide solution into the ferrous sulfate solution at the flow rate of 7mL/min, stirring and reacting for 13min at the rotation speed of 180r/min under the condition of water bath at 17 ℃, dropwise adding 1% sulfuric acid with mass concentration to adjust the pH value to 4.5 to obtain ferrous hydroxide colloid, introducing air into the ferrous hydroxide colloid at the flow rate of 15mL/min for 4min to perform oxidation reaction to obtain an oxidation reactant, adding the oxidation reactant into the deionized water, stirring for 15min at the rotation speed of 220r/min at normal temperature to obtain a mixed solution, adding the sodium silicate solution into the mixed solution, stirring for 350min at the rotation speed of 260r/min at normal temperature, introducing carbon dioxide gas at the air flow rate of 25mL/mim to adjust the pH value to 6.0, filtering out liquid, washing and drying to obtain silicon-coated iron fiber, placing the silicon-coated iron fiber in a 300 ℃ condition for dehydration for 5 hours to obtain a dehydration product, placing the dehydration product in a quartz dish, placing the quartz dish in a reduction furnace, and introducing the quartz dish into the reduction furnace at an air flow rate of 130mL/min and a volume ratio of 1:1, calcining the nitrogen-hydrogen mixed gas at 500 ℃ for 5 hours, and cooling to room temperature along with the furnace to obtain polycrystalline iron fibers; then respectively weighing 90 parts of cotton fiber, 23 parts of polycrystalline iron fiber, 9 parts of silicon carbide fiber and 9 parts of polyacrylonitrile-based carbon fiber according to parts by weight, placing the cotton fiber in an opener, pre-opening for 15min at normal temperature to obtain pre-opened cotton fiber, adding the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber into the pre-opened cotton fiber, placing the pre-opened cotton fiber in a wool-spinning machine, wool-spinning for 25min at normal temperature to obtain mixed fiber, opening and cleaning the mixed fiber at the conditions of the ration of 350g/m and the fixed length of 25m, carding, drawing at the front roller rotating speed of 725r/min to obtain blended fiber, placing the blended and post-added fiber in a roving machine, roving at the roller gauge of 22mm multiplied by 35mm, the rear zone draft multiple of 1, the relative humidity of 80% and the temperature of 25 ℃ at the front roller rotating speed of 250r/min for 30min, and (3) obtaining a coarse spun yarn, placing the coarse spun yarn in a fine spinning machine, performing fine spinning at the speed of a fine yarn spindle of 6100r/min for 35min under the conditions of 50-twist-10 cm, 75% relative humidity and 25 ℃ to obtain a fine spun yarn, placing the fine spun yarn in an automatic bobbin winder, and performing a bobbin winding process at the rotating speed of 875r/min for 1.5h at normal temperature to obtain the wave-absorbing radiation-proof composite textile material.
Example 3
Respectively weighing 50 parts of polydimethylsilane and 120 parts of dimethylbenzene according to parts by weight, placing the polydimethylsilane in a reaction kettle, introducing high-purity nitrogen at an air flow rate of 60mL/min for protection, heating to 200 ℃ at a heating rate of 5 ℃/min, preserving heat for 40min, cooling to normal temperature to obtain a polycarbosilane primary product, adding the polycarbosilane primary product into the dimethylbenzene, stirring at a rotation speed of 400r/min for 30min at normal temperature to obtain a mixed solution, placing the mixed solution under the conditions of a pressure of 400KPa and a temperature of 360 ℃, carrying out reduced pressure distillation for 4, cooling to room temperature to obtain polycarbosilane, placing the polycarbosilane in a melt spinning machine, introducing nitrogen at an air flow rate of 50mL/min for protection, extruding under the conditions of a pressure of 0.4MPa and a temperature of 260 ℃, cooling to room temperature to obtain a polycarbosilane fiber precursor, placing the polycarbosilane fiber precursor in a vertical infusible furnace, heating to 180 ℃ from normal temperature at a heating rate of 5 ℃/min, preserving heat, carrying out non-melting treatment for 30min, cooling to room temperature along with the furnace to obtain non-melting polycarbosilane fiber, putting the fiber into a quartz boat, putting the quartz boat into a corundum tube, introducing nitrogen at an air flow rate of 60mL/min for protection, heating to 1200 ℃ from normal temperature at a heating rate of 5 ℃/min, preserving heat, calcining for 2h, and cooling to room temperature along with the tube to obtain silicon carbide fiber with the average diameter of 0.16 mm; respectively weighing 60 parts by weight of 25% ferrous sulfate solution, 12 parts by weight of 5% sodium hydroxide solution, 30 parts by weight of 10% sodium silicate solution and 120 parts by weight of deionized water, adding the sodium hydroxide solution into the ferrous sulfate solution at the flow rate of 10mL/min, stirring and reacting for 15min at the rotation speed of 200r/min under the condition of water bath at 20 ℃, dropwise adding 1% sulfuric acid at the mass concentration to adjust the pH value to 5 to obtain a ferrous hydroxide colloid, introducing air into the ferrous hydroxide colloid at the flow rate of 20mL/min for 5min to perform oxidation reaction to obtain an oxidation reactant, adding the oxidation reactant into the deionized water, stirring for 20min at the rotation speed of 240r/min at normal temperature to obtain a mixed solution, adding the sodium silicate solution into the mixed solution, stirring for 40min at the rotation speed of 280r/min at normal temperature, introducing carbon dioxide gas at the air flow rate of 30mL/mim to adjust the pH value to 6.2, filtering out liquid, washing and drying to obtain silicon-coated iron fiber, dehydrating the silicon-coated iron fiber for 6 hours at 400 ℃ to obtain a dehydrated product, putting the dehydrated product into a quartz dish, putting the quartz dish into a reduction furnace, and introducing the dehydrated product into the reduction furnace at an air flow rate of 140mL/min and a volume ratio of 1:1, calcining the nitrogen-hydrogen mixed gas at 600 ℃ for 6 hours, and cooling to room temperature along with the furnace to obtain polycrystalline iron fibers; then weighing 100 parts of cotton fiber, 25 parts of polycrystalline iron fiber, 10 parts of silicon carbide fiber and 10 parts of polyacrylonitrile-based carbon fiber respectively according to parts by weight, placing the cotton fiber in an opener, pre-opening for 20min at normal temperature to obtain pre-opened cotton fiber, adding the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber into the pre-opened cotton fiber, placing the pre-opened cotton fiber in a wool-spinning machine, wool-spinning for 30min at normal temperature to obtain mixed fiber, opening and cleaning the mixed fiber at the conditions of a fixed quantity of 400g/m and a fixed length of 30m, carding, drawing at a front roller rotating speed of 750r/min to obtain blended fiber, placing the blended and post-added fiber in a roving machine, roving at a front roller rotating speed of 300r/min for 40min under the conditions of a roller gauge of 22mm multiplied by 35mm, a rear zone drafting multiple of 1, a relative humidity of 80% and a temperature of 25 ℃, and (3) obtaining a coarse spun yarn, placing the coarse spun yarn in a fine spinning machine, performing fine spinning for 40min at the spun yarn spindle speed of 6200r/min under the conditions of 50-cm twist for fixed twist, 75% relative humidity and 25 ℃ to obtain a fine spun yarn, placing the fine spun yarn in an automatic bobbin winder, and performing a bobbin winding process for 2h at the rotating speed of 900r/min at normal temperature to obtain the wave-absorbing and radiation-proof composite textile material.
The wave-absorbing radiation-proof composite textile material prepared by the invention and the commercially available wave-absorbing textile material are detected, and the specific detection results are shown in the following table 1:
4 samples of the materials of examples 1 to 3 and comparative example were cut out and measured by the bow method which is commonly used internationally. The reflectivity dB was measured in this experiment using an agilent vector network analyzer (agilent f5230 c). The testing frequency range is 2-18 GHZ, and the average value of each fabric is obtained by two times of front side testing. When the reflectivity dB is a negative value, the smaller the dB value is, the better the wave absorbing performance is; the larger the dB value is, the poorer the wave absorbing performance is; using YG461E air permeability tester, according to GBJT 5453: 1997. The test specimen specification was l0cm × l0cm, the pressure difference of the test specimen of the industrial fabric was set to 200Pa, and each fabric was tested 5 times per specimen and averaged, and the specific test results are shown in table 1 below.
Table 1 wave-absorbing radiation-proof composite textile material property characterization
From table 1, it can be seen that the wave-absorbing radiation-proof composite textile material prepared by the invention has good wave-absorbing performance, good air permeability and strong comfort.
Claims (3)
1. A preparation method of a wave-absorbing radiation-proof composite textile material is characterized by comprising the following specific preparation steps:
(1) placing the cotton fibers in an opener, and pre-opening for 10-20 min at normal temperature to obtain pre-opened cotton fibers;
(2) adding polycrystalline iron fibers, silicon carbide fibers and polyacrylonitrile-based carbon fibers into pre-opened cotton fibers, placing the cotton fibers in a wool blending machine, and blending for 20-30 min at normal temperature to obtain mixed fibers; the weight parts of the cotton fiber, the polycrystalline iron fiber, the silicon carbide fiber and the polyacrylonitrile-based carbon fiber are 80-100 parts of the cotton fiber, 20-25 parts of the polycrystalline iron fiber, 8-10 parts of the silicon carbide fiber and 8-10 parts of the polyacrylonitrile-based carbon fiber;
the preparation method of the polycrystalline iron fiber comprises the following specific steps:
a. adding a sodium hydroxide solution into a ferrous sulfate solution at a flow rate of 5-10 mL/min, stirring and reacting for 10-15 min at a rotation speed of 160-200 r/min under a water bath condition of 15-20 ℃, dropwise adding sulfuric acid with a mass concentration of 1% to adjust the pH to 4-5, and obtaining a ferrous hydroxide colloid;
b. introducing air into the ferrous hydroxide colloid at a flow rate of 10-20 mL/min for 3-5 min for oxidation reaction to obtain an oxidation reactant;
c. adding the oxidation reactant into deionized water, and stirring at the rotating speed of 200-240 r/min for 10-20 min at normal temperature to obtain a mixed solution;
d. adding a sodium silicate solution into the mixed solution, stirring at the normal temperature at the rotating speed of 240-280 r/min for 30-40 min, introducing carbon dioxide gas at the air flow speed of 20-30 mL/mim to adjust the pH value to 5.8-6.2, filtering out liquid, washing, and drying to obtain silicon-coated iron fibers;
e. dehydrating the silicon-coated iron fiber for 4-6 hours at the temperature of 200-400 ℃ to obtain a dehydrated product;
f. placing the dehydrated product into a quartz vessel, placing the quartz vessel into a reduction furnace, introducing nitrogen-hydrogen mixed gas, calcining for 4-6 hours at the temperature of 400-600 ℃, and cooling to room temperature along with the furnace to obtain polycrystalline iron fibers; the volume ratio of nitrogen to hydrogen in the nitrogen-hydrogen mixed gas is 1:1, and the gas introduction speed is 120-140 mL/min;
the silicon carbide fiber is prepared by the following specific steps:
placing polydimethylsiloxane into a reaction kettle, introducing high-purity nitrogen at the air flow rate of 40-60 mL/min for protection, heating to 200 ℃ at the heating rate of 5 ℃/min, preserving heat for 20-40 min, and cooling to normal temperature to obtain a polycarbosilane primary product;
II, adding the polycarbosilane primary product into dimethylbenzene, and stirring at the rotating speed of 300-400 r/min for 20-30 min at normal temperature to obtain a mixed solution;
III, placing the mixed solution under the conditions of the pressure of 300-400 KPa and the temperature of 340-360 ℃ for reduced pressure distillation for 2-4, and cooling to room temperature to obtain polycarbosilane;
putting polycarbosilane in a melt spinning machine, introducing nitrogen at the air flow rate of 40-50 mL/min for protection, extruding under the conditions of the pressure of 0.2-0.4 MPa and the temperature of 240-260 ℃, and cooling to room temperature to obtain polycarbosilane fiber precursor;
placing the polycarbosilane fiber precursor in a vertical non-melting furnace, heating the polycarbosilane fiber precursor to 180 ℃ from normal temperature at the heating rate of 3-5 ℃/min, preserving the heat, performing non-melting treatment for 20-30 min, and cooling the polycarbosilane fiber precursor to room temperature along with the furnace to obtain non-melting polycarbosilane fiber;
putting the fiber into a quartz boat, putting the quartz boat into a corundum tube, introducing nitrogen at the air flow rate of 40-60 mL/min for protection, heating the quartz boat to 1200 ℃ from the normal temperature at the heating rate of 5 ℃/min, carrying out heat preservation calcination for 1-2 h, and cooling the quartz boat to the room temperature along with the tube to obtain the silicon carbide fiber with the average diameter of 0.12-0.16 mm;
(3) opening and picking the mixed fibers, then drawing the mixed fibers at the rotating speed of a front roller of 700-750 r/min after a cotton carding process to obtain the blended fibers; the conditions of the opening and picking process are that the ration is 300-400 g/m, and the fixed length is 20-30 m;
(4) putting the fibers which are added in the spinning process into a roving machine, and performing roving at the rotating speed of a front roller of 200-300 r/min for 20-40 min to obtain a roving yarn; the conditions of the roving are that the roller gauge is 22mm multiplied by 35mm, the drafting multiple of the rear zone is 1, the relative humidity is 80 percent and the temperature is 25 ℃;
(5) putting the rough spun yarn into a fine spinning machine, and fine spinning at the spun yarn spindle speed of 6000-6200 r/min for 30-40 min to obtain fine spun yarn; the conditions of the fine spinning are that the twist is 50 twist/10 cm, the relative humidity is 75 percent, and the temperature is 25 ℃;
(6) and (3) placing the fine spun yarns in an automatic winder, and performing a winding process for 1-2 hours at the rotating speed of 850-900 r/min at normal temperature to obtain the radiation-proof composite textile material.
2. The preparation method of the wave-absorbing radiation-proof composite textile material according to claim 1, wherein the weight parts of the ferrous sulfate solution, the sodium hydroxide solution, the sodium silicate solution and 100 to 120 parts of deionized water are 50 to 60 parts of 25 mass percent ferrous sulfate solution, 10 to 12 parts of 5 mass percent sodium hydroxide solution, 20 to 30 parts of 10 mass percent sodium silicate solution and 100 to 120 parts of deionized water.
3. The preparation method of the wave-absorbing radiation-proof composite textile material according to claim 1, wherein the weight parts of the polydimethylsilane and the xylene are 40-50 parts of the polydimethylsilane and 100-120 parts of the xylene.
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