CN114541138A - Rare earth-based infrared heating warm-keeping fabric and preparation method and application thereof - Google Patents

Rare earth-based infrared heating warm-keeping fabric and preparation method and application thereof Download PDF

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CN114541138A
CN114541138A CN202210436412.4A CN202210436412A CN114541138A CN 114541138 A CN114541138 A CN 114541138A CN 202210436412 A CN202210436412 A CN 202210436412A CN 114541138 A CN114541138 A CN 114541138A
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rare earth
parts
yarn
infrared heating
heat transfer
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CN114541138B (en
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邓冠南
李璐
方纾
彭维
张光睿
成颖
刘金龙
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Tianjin Baogang Rare Earth Research Institute Co Ltd
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Tianjin Baogang Rare Earth Research Institute Co Ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/026—Knitted fabric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/78—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon; with halides or oxyhalides of silicon; with fluorosilicates
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    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/507—Polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B32B2262/062—Cellulose fibres, e.g. cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B32B2262/062—Cellulose fibres, e.g. cotton
    • B32B2262/065—Lignocellulosic fibres, e.g. jute, sisal, hemp, flax, bamboo
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/08—Animal fibres, e.g. hair, wool, silk
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2437/00—Clothing
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention provides a rare earth-based infrared heating warm-keeping fabric and a preparation method and application thereof. The rare earth-based infrared heating warm-keeping fabric provided by the invention is simple in structure, the manufacturing cost of the traditional heating element warm-keeping clothes is obviously reduced, and the fabric is convenient to clean.

Description

Rare earth-based infrared heating warm-keeping fabric and preparation method and application thereof
Technical Field
The invention belongs to the technical field of textile fabrics, and particularly relates to a rare earth-based infrared heating warm-keeping fabric, and a preparation method and application thereof.
Background
The heat loss mode comprises three modes of heat conduction, heat convection and heat radiation, and at present, the conventional method of the warm-keeping clothes in the market utilizes the filling power of down or cotton to stop the flow of air, prevent the quick loss of heat of the machine body and achieve the effect of keeping warm. The method can only reduce the loss of heat and can not actively provide warm for the body. With the progress of textile technology and science and technology, in order to further improve the warm-keeping effect of clothes, the heating elements are added on the clothes and connected through various leads, so that the heating effect is maintained by the batteries, for example, in patent CN201420501751.7, "constant temperature warm-keeping clothes and warm-keeping circuit using lithium batteries", a PWM/PFM control module is used to realize constant temperature control, that is, when the temperatures of the two electric heating sheets rise to a set temperature, the current flowing through the two electric heating sheets or the working states of the two electric heating sheets are controlled by a field effect transistor, so as to realize the constant temperature of the two electric heating sheets, and further realize the constant temperature of the warm-keeping clothes. But this way makes the winter clothes that are inherently bulky thicker and heavier. The thermal clothes need to disassemble the power supply part or cannot be washed by water, so that the inconvenience of washing is brought.
Disclosure of Invention
In view of the above, the invention provides a rare earth-based infrared heating warm-keeping fabric, and a preparation method and application thereof, aiming at overcoming the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a rare earth-based infrared heating warm-keeping fabric comprises a heating layer and a heat transfer warm-keeping layer, wherein the heating layer is formed by weaving rare earth-based infrared heating yarns, the rare earth-based infrared heating yarns are prepared by impregnating yarns with rare earth-based infrared heating impregnating solution, the heat transfer warm-keeping layer is formed by weaving rare earth-based heat transfer yarns, and the rare earth-based heat transfer yarns are prepared by impregnating yarns with rare earth-based high-heat-transfer impregnating solution;
the rare earth-based infrared heating impregnation liquid contains 0.1-30 wt% of rare earth-based infrared heating slurry, and the rare earth-based infrared heating slurry comprises the following raw materials in parts by weight: 10-30 parts of near-infrared absorption powder, 45-99 parts of dispersion medium A and 1-15 parts of dispersing agent A, wherein the near-infrared absorption powder comprises 16-60 parts by weight of rare earth hexaboride and 40-84 parts by weight of cesium tungsten bronze, the rare earth hexaboride comprises 5-20 parts by weight of lanthanum hexaboride and 5-10 parts by weight of CexLa1-xB61-10 parts by weight of SmxLa1-xB65-10 parts by weight of EuxLa1-xB60-5 parts by weight of GdxLa1-xB60 to 5 parts by weight of YxLa1-xB6Wherein X is 0.1-0.9;
the rare earth-based high heat transfer impregnating solution contains 0.1-60 wt% of rare earth-based high heat transfer slurry, and the rare earth-based high heat transfer slurry comprises the following raw materials in parts by weight: 30-60 parts of heat transfer powder, 45-99 parts of dispersion medium B and 10-25 parts of dispersing agent B, wherein the heat transfer powder comprises 1-15 parts of yttrium zirconium oxide, 10-30 parts of lanthanum cerium oxide, 10-30 parts of lanthanum samarium oxide, 20-40 parts of silicon carbide and 20-40 parts of carbon black composite graphene.
Preferably, the particle size distribution of the near-infrared absorption powder is 50-130nm, and the particle size distribution of the heat transfer powder is 200-450 nm.
Preferably, the dispersion medium A and the dispersion medium B are respectively and independently selected from one or more of deionized water, ethanol, ethylene glycol, propylene glycol methyl ether acetate, ethylene glycol butyl ether acetate, polymethyl methacrylate, dimethyl succinate, dimethyl glutarate and ethyl acetate.
Preferably, the dispersant A and the dispersant B are both independently selected from one or more of sodium hexametaphosphate, sodium tripolyphosphate, sodium benzenesulfonate, azalidine, acetylenic diol, polyamide wax, polyolefin wax, polycarbodiimide, hydrogenated lecithin, N-methylpyrrolidone solution of modified polyurea, and cymene diol.
Preferably, the heat generating layer and the heat transfer and warm keeping layer are independently selected from single-sided fabric, double-sided fabric or spacer fabric.
Preferably, the yarn materials of the heating layer and the heat transfer warm-keeping layer are selected from cotton fabrics, hemp fabrics, wool fabrics, silk fabrics and chemical fibers independently.
Preferably, the yarn density of the heat-generating layer is 5-10 times of that of the heat-transfer warm-keeping layer.
The invention also provides a preparation method of the rare earth-based infrared heating yarn, which comprises the following steps:
the method comprises the following steps: uniformly mixing 0.1-30 wt% of rare earth-based infrared heating material slurry, 1-10 wt% of adhesive and 1-5 wt% of flatting and softening agent in a high-speed dispersion machine, and injecting the mixture into an impregnation tank;
step two: soaping the yarn in 35-45 ℃ water bath for 5-12min, dehydrating and drying at 80-85 ℃ for 3-7 min;
step three: cleaning, and then conveying the mixture into a dipping pool for dipping at the pH value of 7.5-8.5 and the dipping temperature of 65-75 ℃, wherein the dipping time is 5-7min, and the rolling allowance rate is 75-85%;
step four: secondary impregnation, wherein the impregnation temperature is 95-99 ℃, the impregnation time is 1-3min, the rolling residue rate is 65-75%, the drying temperature is 90-120 ℃, and the drying time is 55-75 s;
step five: transferring the mixture into a 3-7% polyester solution pool, soaking the mixture for 45-65s at the temperature of 35-55 ℃ in the pool, and drying the mixture for 3-7min at the temperature of 80-85 ℃ to obtain the rare earth-based infrared heating yarn.
The invention also provides a preparation method of the rare earth-based heat transfer yarn, which comprises the following steps:
the method comprises the following steps: uniformly mixing 0.1-60 wt% of rare earth-based high-heat-transfer slurry, 1-10 wt% of adhesive and 1-5 wt% of flatting agent in a high-speed dispersion machine, and injecting the mixture into an impregnation tank;
step two: soaping the yarn in 35-45 ℃ water bath for 5-12min, dehydrating and drying at 80-85 ℃ for 3-7 min;
step three: cleaning, and then conveying the mixture into a dipping pool for dipping at the pH value of 7.5-8.5 and the dipping temperature of 65-75 ℃, wherein the dipping time is 5-7min, and the rolling allowance rate is 75-85%;
step four: secondary impregnation, wherein the impregnation temperature is 95-99 ℃, the impregnation time is 1-3min, the rolling residue rate is 65-75%, the drying temperature is 90-120 ℃, and the drying time is 55-75 s;
step five: transferring the mixture into a 3-7% polyester solution pool, soaking the mixture for 45-65s at the temperature of 35-55 ℃ in the pool, and drying the mixture for 3-7min at the temperature of 80-85 ℃ to obtain the rare earth-based heat transfer yarn.
The invention also provides application of the rare earth-based infrared heating warm-keeping fabric in the fields of clothing and home textiles.
The invention also provides a preparation method of the rare earth-based infrared heating warm-keeping fabric, which comprises the following steps: the rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure, and a warp knitting layer woven by the front needle bed and the back needle bed drives the rare earth-based heat transfer yarn to connect a heating layer with a heat transfer and insulation layer through a yarn guide comb.
Compared with the prior art, the invention has the following advantages:
(1) the rare earth-based infrared heating material has a Local Surface Plasma Resonance (LSPR) effect of free electrons, has an obvious absorption effect on near-infrared radiation in sunlight, and the infrared ray occupies nearly 50% of energy in the sunlight. In the solar spectrum, lanthanum hexaboride mainly absorbs 780-1300nm near infrared rays; the special lanthanum cerium hexaboride in the invention mainly absorbs the near infrared ray of 800-1350 nanometers, and the samarium hexaboride, europium hexaboride, gadolinium hexaboride and yttrium hexaboride mainly absorb the near infrared ray of 800-1500 nanometers. The cesium tungsten bronze (TTO) mainly absorbs near infrared rays of 900-. Therefore, the rare earth-based infrared absorption material and the TTO material play a role in near-infrared cooperative absorption on the near-infrared spectrum, and make up for the near-infrared absorption defect. The heating layer formed by warp knitting rare earth-based infrared heating yarns converts radiation heat energy into physical heat energy to be adsorbed on the surface of the fabric, so that a self-heating effect is achieved, the rare earth-based heat transfer material endows the heat transfer yarns with excellent heat conduction performance, the structural density of the heat transfer warm-keeping layer is dense outside and sparse inside, the heat transfer connecting lines are tight outside and loose inside, the internal temperature is reduced, and heat flux is transferred to the heating layer, so that the heat transfer warm-keeping effect is achieved. Under the illumination condition, the temperature of the added rare earth-based infrared heating fabric layer is effectively increased by 2-7 ℃ compared with the temperature of the fabric which is not added.
(2) According to the invention, the rare earth-based infrared heating material slurry is attached to the yarns through a dipping technology and is warp-knitted to form the heating layer, and the heating and warming effects are achieved by matching with the heat transfer warming layer.
(3) The rare earth-based infrared heating warm-keeping fabric provided by the invention is simple in structure, the manufacturing cost of the traditional heating element warm-keeping clothes is obviously reduced, and the fabric is convenient to clean.
Drawings
FIG. 1 is a diagram showing a transmittance spectrum of a near-infrared absorbing powder;
FIG. 2 is an X-ray diffraction pattern of the near-infrared absorbing powder.
Detailed Description
Unless defined otherwise, technical terms used in the following examples and comparative examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. Lanthanum hexaboride and TTO used in the following examples and comparative examples are commercially available, the yarn is made of cotton yarn, and other reagents are conventional biochemical reagents unless otherwise specified; the experimental methods are all conventional methods unless otherwise specified, and fig. 1 is a transmittance spectrum of the near-infrared absorption powder, and fig. 2 is an X-ray diffraction spectrum of the near-infrared absorption powder. The sources and grades of the other raw materials in the slurry are:
cesium tungsten bronze: tianjin Bao rare earth institute purchase brand TTO20211231 CN;
lanthanum hexaboride: the Baotou rare earth research institute purchases L material 202110 LF; yttrium zirconium oxide: commercially available SEPR 9503;
and (3) lanthanum cerium oxide: the commercial Baotou rare earth institute hydrometallurgy department;
samarium lanthanum oxide: the commercial Baotou rare earth institute hydrometallurgy department;
silicon carbide: commercial technical grade 40921-2;
carbon black composite graphene: tinocon is a commercial industrial grade.
The invention will be described in detail with reference to the following examples.
Examples 1 to 5 preparation of binary rare earth-based hexaboride
EXAMPLE 1 preparation of Gd0.1La0.9B6A powder comprising the steps of:
(1) according to the Gd: la: b: na: SiO 22The molar ratio is 0.1:0.9:6:24:12, Gd is weighed respectively2(CO3）3495g，La2（CO3）3 2060g，B2O3 2089g，Na 552g，SiO2720g, all raw materials are put into a high-pressure reaction kettle, 12 mol of hydrogen is introduced, the temperature is heated to 320 ℃, and the mixture is stirred for two hours. Extracting and layering the obtained product by using deionized water, carrying out suction filtration and washing on the precipitate for 5 times, and drying the obtained product for 5 hours at 110 ℃. And (3) putting the dried product and 6 kg of deionized water into a sand mill, grinding for 8 hours, testing to obtain slurry with the granularity of 700 nm, and performing first spray granulation and drying on the slurry to obtain powder with the granularity of 800 nm, wherein the first spray granulation is performed on the slurry. Carrying out secondary airflow milling, grinding and granulation on the 700-plus-800 nanometer powder to obtain a precursor of the 150-plus-130 nanometer powder, and filling the precursor into a rotary furnace, wherein the filling height of the precursor is 3 cm;
(2) and (3) introducing 10% hydrogen-nitrogen mixed gas into the rotary furnace after the material is sealed, wherein the speed is 100ml/min for 1min, and then starting to heat. A first temperature rise stage: the room temperature is 200 ℃, the aeration rate is 2ml/min, the inclination angle of the rotary furnace is 15 ℃, and the rotation speed is 10 rpm; a second temperature rising stage: from 200 ℃ to 490 ℃, the aeration rate is 5ml/min, the rotary kiln is tilted at 10 ℃ and the rotation rate is 10 rpm. Preserving the heat for 10 min; a third temperature rise stage: after the temperature is increased from 490 ℃ to 870 ℃, the aeration rate is 30ml/min, the inclination angle of the rotary kiln is 3 ℃, and the rotation speed is 30 rpm. The heating rate of the first and second heating stages is 7 ℃/min, and the heating rate of the third heating stage is 3 ℃/min. And (3) heat preservation, wherein the first temperature rise stage is used for preserving heat for 30min when reaching 200 ℃. And preserving the heat for 30min when the temperature of the second temperature rise stage reaches 490 ℃. And preserving the heat for 150min when the temperature of the third temperature rise stage reaches 870 ℃. A temperature reduction process, wherein in the first temperature reduction stage, the temperature is reduced from 850 ℃ to 490 ℃, the aeration rate is 30ml/min, and the rotation rate is 30 rpm; and a second cooling stage: the temperature was lowered from 490 ℃ to room temperature, the aeration rate was 2ml/min and the rotation rate was 10 rpm. The temperature reduction rate of the first temperature reduction stage is 15 ℃/min, the second temperature reduction stage is air-cooled along with the furnace, and the initial product can be obtained after the temperature is reduced to the room temperature.
(3) Washing the initial product with 5mol/L hydrochloric acid and deionized water until the washing solution is dripped with AgNO3No precipitation is generated in the solution to obtain a dark green reduction product Gd0.1La0.9B6。
Example 2 preparation of Ce0.1La0.9B6Powder, according to Ce: la: b: na: SiO 22The molar ratio of Ce (NO) to Ce (NO) was measured at 0.1:0.9:6:24:123)3 326g，La2（CO3）3 2060g，B2O3 2089g，Na 552g，SiO2 720g, the rest steps and 1.1 preparing Gd0.1La0.9B6The powder steps are the same.
EXAMPLE 3 preparation of Sm0.1La0.9B6Powder, according to Sm: la: b: na: SiO 22Sm (NO) is weighed according to the molar ratio of 0.1:0.9:6:24:123)3 336g，La2（CO3）3 2060g，B2O3 2089g，Na 552g，SiO2 720g, the rest of the steps are combined with 1.1 for preparing Gd0.1La0.9B6The powder steps are the same.
Example 4 preparation of Y0.1La0.9B6Powder, according to Y: la: b: na: SiO 22The molar ratio is 0.1:0.9:6:24:12, and Y is weighed respectively(NO3)3 383g，La2（CO3）3 2060g，B2O3 2089g，Na 552g，SiO2 720g, the rest of the steps and 1.1 preparing Gd0.1La0.9B6The powder steps are the same.
EXAMPLE 5 preparation of Eu0.1La0.9B6Powder, according to Eu: la: b: na: SiO 22The molar ratio of EuCl to EuCl was 0.1:0.9:6:24:123 258g，La2（CO3）3 2060g，B2O3 2089g，Na 552g，SiO2 720g, the rest steps and 1.1 preparing Gd0.1La0.9B6The powder steps are the same.
The transmittance spectra of the five binary rare earth hexaborides prepared in example 1 and lanthanum hexaboride and cesium tungsten bronze were measured using an ultraviolet-visible-near infrared spectrophotometer (model: DUV-3700) using the binary rare earth hexaboride and lanthanum hexaboride and cesium tungsten bronze prepared in examples 1, and as shown in FIG. 1, it can be seen that the binary rare earth hexaboride and lanthanum hexaboride and cesium tungsten bronze have high absorption in the near infrared region (wavelength 780-2500 nm).
Examples 6-8 and comparative examples 1-4 rare earth based infrared heating thermal fabrics were prepared in which the binary rare earth based hexaboride compounds used were all prepared in examples 1-5.
Example 6
Taking 5 parts of 130 nanoscale lanthanum hexaboride, 5 parts of cerium hexaboride, 1 part of samarium hexaboride, 5 parts of europium hexaboride, 2 parts of gadolinium lanthanum hexaboride, 2 parts of yttrium lanthanum hexaboride, 80 parts of TTO, 90 parts of deionized water-ethanol mixed solution (the volume ratio is 90: 10), and 4 parts of N-methylpyrrolidone and hydrogenated lecithin mixed solution (the volume ratio is 90: 10) of modified polyurea, fully and uniformly mixing to obtain rare earth-based infrared heating slurry, and injecting the 92wt% rare earth-based infrared heating slurry, 5wt% adhesive and 3wt% smoothing agent into a dipping tank after uniformly mixing in a high-speed dispersion machine, wherein the solid content of the dipping tank is 10%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, drying at 110 ℃ for 55-75 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn.
Fully and uniformly mixing 5 parts of 400-nanoscale yttrium zirconium oxide, 30 parts of lanthanum cerium oxide, 20 parts of lanthanum samarium oxide, 10 parts of silicon carbide, 35 parts of carbon black composite graphene, 70 parts of deionized water-ethanol mixed liquor, 10 parts of sodium hexametaphosphate and polyolefin wax mixed liquor (the volume ratio is 90: 10) to obtain rare earth-based high heat transfer slurry, uniformly mixing 92wt% of rare earth-based high heat transfer slurry, 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine, and injecting the mixture into a dipping tank. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 5 times of that of the warp knitting yarns of the heat transfer and insulation layer.
Example 7
Taking 8 parts of 120 nanoscale lanthanum hexaboride, 5 parts of cerium hexaboride, 3 parts of samarium hexaboride, 8 parts of europium hexaboride, 2 parts of gadolinium lanthanum hexaboride, 2 parts of yttrium lanthanum hexaboride, 72 parts of TTO, 80 parts of deionized water-ethanol mixed solution (the volume ratio is 90: 10), and 5 parts of N-methyl pyrrolidone and hydrogenated lecithin mixed solution (the volume ratio is 90: 10) of modified polyurea, fully and uniformly mixing to obtain rare earth-based infrared heating slurry, and injecting the 92wt% rare earth-based infrared heating slurry, 5wt% adhesive and 3wt% smoothing agent into an impregnation tank after uniformly mixing in a high-speed dispersion machine, wherein the solid content of the impregnation tank is 20%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn.
Fully mixing 5 parts of 400-nanoscale yttrium zirconium oxide, 30 parts of lanthanum cerium oxide, 20 parts of lanthanum samarium oxide, 10 parts of silicon carbide, 35 parts of carbon black composite graphene, 70 parts of deionized water-ethanol mixed liquor (the volume ratio is 90: 10), 10 parts of sodium hexametaphosphate and polyolefin wax mixed liquor (the volume ratio is 90: 10) uniformly, mixing 92wt% of rare earth-based high heat transfer slurry, 5wt% of adhesive and 3wt% of smoothing agent uniformly in a high-speed dispersion machine, and injecting the mixture into a dipping tank. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary dipping, wherein the pH is 7.5, the dipping is carried out for 1min at 95 ℃, the rolling residue rate is 65 percent, and the drying is carried out for 55s at 110 ℃. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 6 times of that of the heat transfer warm-keeping layer.
Example 8
Taking 10 parts of 110 nanoscale lanthanum hexaboride, 6 parts of lanthanum cerium hexaboride, 3 parts of lanthanum samarium hexaboride, 10 parts of lanthanum europium hexaboride, 3 parts of lanthanum gadolinium hexaboride, 3 parts of lanthanum yttrium hexaboride, 65 parts of TTO, 70 parts of deionized water-ethanol mixed solution (the volume ratio is 90: 10), 12 parts of N-methyl pyrrolidone and hydrogenated lecithin mixed solution (the volume ratio is 90: 10) of modified polyurea, fully and uniformly mixing to obtain rare earth-based infrared heating slurry, uniformly mixing 92wt% of the rare earth-based infrared heating slurry, 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine, and then injecting the mixture into an impregnation tank, wherein the solid content of the impregnation tank is 30%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn.
Fully mixing 5 parts of 400-nanoscale yttrium zirconium oxide, 30 parts of lanthanum cerium oxide, 20 parts of lanthanum samarium oxide, 10 parts of silicon carbide, 35 parts of carbon black composite graphene, 70 parts of deionized water-ethanol mixed liquor (the volume ratio is 90: 10), 10 parts of sodium hexametaphosphate and polyolefin wax mixed liquor (the volume ratio is 90: 10) uniformly, mixing 92wt% of rare earth-based high heat transfer slurry, 5wt% of adhesive and 3wt% of smoothing agent uniformly in a high-speed dispersion machine, and injecting the mixture into a dipping tank. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 8 times of that of the heat transfer warm-keeping layer.
Example 9
Taking 10 parts of 110 nanoscale lanthanum hexaboride, 6 parts of lanthanum cerium hexaboride, 3 parts of lanthanum samarium hexaboride, 10 parts of lanthanum europium hexaboride, 71 parts of TTO, 70 parts of deionized water-ethanol mixed solution (volume ratio of 90: 10), 12 parts of modified polyurea N-methyl pyrrolidone and hydrogenated lecithin mixed solution (volume ratio of 90: 10), fully and uniformly mixing to obtain rare earth-based infrared heating slurry, uniformly mixing 92wt% of the rare earth-based infrared heating slurry, 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine, and injecting the mixture into a dipping tank, wherein the solid content of the dipping tank is 30%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 for 7min at 65 deg.C, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn.
Fully mixing 5 parts of 400-nanoscale yttrium zirconium oxide, 30 parts of lanthanum cerium oxide, 20 parts of lanthanum samarium oxide, 10 parts of silicon carbide, 35 parts of carbon black composite graphene, 70 parts of deionized water-ethanol mixed liquor (the volume ratio is 90: 10), 10 parts of sodium hexametaphosphate and polyolefin wax mixed liquor (the volume ratio is 90: 10) uniformly, mixing 92wt% of rare earth-based high heat transfer slurry, 5wt% of adhesive and 3wt% of smoothing agent uniformly in a high-speed dispersion machine, and injecting the mixture into a dipping tank. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 8 times of that of the heat transfer warm-keeping layer.
COMPARATIVE EXAMPLE 1 (No Heat transfer Warm-keeping layer)
The preparation method comprises the following steps of taking 5 parts of 130 nanoscale lanthanum hexaboride, 5 parts of cerium lanthanum hexaboride, 1 part of samarium hexaboride, 5 parts of europium lanthanum hexaboride, 2 parts of gadolinium lanthanum hexaboride, 2 parts of yttrium lanthanum hexaboride, 80 parts of TTO, 90 parts of deionized water-ethanol mixed solution (the volume ratio is 90: 10), 4 parts of N-methyl pyrrolidone and hydrogenated lecithin (the volume ratio is 90: 10) mixed solution of modified polyurea, fully mixing uniformly rare earth-based infrared heating slurry, mixing uniformly 92wt% of rare earth-based infrared heating slurry, 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine, and injecting the mixture into a dipping tank, wherein the solid content of the dipping tank is 10%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to make a warp flat structure, and the common yarn is loaded into a back needle bed of the warp knitting machine to make a warp flat structure. The warp knitting layers woven by the front needle bed and the back needle bed drive common yarns to connect the two layers of structures through the yarn guide comb. The spinning density of the common yarn layer is the same as that of the heating layer.
Comparative example 2 (rare earth base-free compound infrared heating slurry)
100 parts of 130 nano TTO, 90 parts of deionized water and ethanol mixed solution, 4 parts of N-methylpyrrolidone of modified polyurea and hydrogenated lecithin mixed solution (the volume ratio is 90: 10) are fully and uniformly mixed to obtain dipping slurry, 92wt% of the slurry, 5wt% of adhesive and 3wt% of flatting agent are uniformly mixed in a high-speed dispersion machine and then injected into a dipping tank, and the solid content concentration of the dipping tank is 10%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, drying at 110 ℃ for 55-75 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the infrared heating yarn.
Fully and uniformly mixing 400 nanometer yttrium zirconium oxide 5 parts, lanthanum cerium oxide 30 parts, lanthanum samarium oxide 20 parts, silicon carbide 10 parts, carbon black composite graphene 35 parts, deionized water-ethanol mixed liquor (volume ratio is 90: 10) 70 parts, sodium hexametaphosphate and polyolefin wax mixed liquor (volume ratio is 90: 10) 10 parts, uniformly mixing rare earth-based high heat transfer slurry 92wt%, adhesive 5wt% and flatting agent 3wt%, and then injecting the mixture into a dipping pool. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 5 times of that of the heat transfer warm-keeping layer.
Comparative example 3
65 parts of 130 nano-scale lanthanum hexaboride, 35 parts of TTO, 90 parts of a deionized water ethanol mixed solution, 4 parts of a modified polyurea N-methyl pyrrolidone and hydrogenated lecithin mixed solution are fully and uniformly mixed, 92wt% of rare earth based infrared heating slurry, 5wt% of adhesive and 3wt% of smoothing agent are uniformly mixed in a high-speed dispersion machine and then injected into a dipping pool, and the solid content concentration of the dipping pool is 10%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 for 7min at 65 deg.C, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, drying at 110 ℃ for 55-75 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ in the pool, and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based infrared heating yarn.
Fully and uniformly mixing 5 parts of 400-nanoscale yttrium zirconium oxide, 30 parts of lanthanum cerium oxide, 20 parts of lanthanum samarium oxide, 10 parts of silicon carbide, 35 parts of carbon black composite graphene, 70 parts of deionized water-ethanol mixed solution, 10 parts of sodium hexametaphosphate and 10 parts of polyolefin wax, uniformly mixing 92wt% of rare earth-based high heat transfer slurry, 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine, and then injecting the mixture into a dipping pool. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. And (3) transferring the yarn into a 3% polyester solution pool, soaking the yarn for 45s at the temperature of 45 ℃ and drying the yarn for 7min at the temperature of 85 ℃ to obtain the rare earth-based heat transfer yarn. The rare earth-based infrared heating yarn is loaded into a front needle bed of a warp knitting machine to form a warp flat structure, and the rare earth-based heat transfer yarn is loaded into a back needle bed of the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed drive the rare earth-based heat transfer yarns to connect the heating layer with the heat transfer warm-keeping layer through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 5 times of that of the heat transfer warm-keeping layer.
Comparative example 4
90 parts of deionized water and ethanol mixed solution and 4 parts of N-methylpyrrolidone and hydrogenated lecithin mixed solution (the volume ratio is 90: 10) of the modified polyurea are fully and uniformly mixed to prepare slurry, and the slurry, 5wt% of adhesive and 3wt% of smoothing agent are uniformly mixed in a high-speed dispersion machine and then injected into a dipping tank, wherein the solid content of the dipping tank is 10%. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, drying at 110 ℃ for 55-75 s. Transferring into a 3% polyester solution tank, soaking at 45 deg.C for 45s, and oven drying at 85 deg.C for 7min to obtain inner layer yarn.
70 parts of deionized water-ethanol mixed solution (volume ratio is 90: 10) and 10 parts of sodium hexametaphosphate and polyolefin wax mixed solution (volume ratio is 90: 10) are fully and uniformly mixed, and the mixture is uniformly mixed with 5wt% of adhesive and 3wt% of smoothing agent in a high-speed dispersion machine and then injected into a dipping tank. The solid content of the dipping pool is 30 percent. The yarn is soaped by water bath at 35 ℃ for 8min, dehydrated and dried, and dried at 85 ℃ for 5 min. Cleaning, soaking in a soaking tank at pH7.5 at 65 deg.C for 7min, and rolling residue rate of 85%. Secondary impregnation, pH7.5, impregnation at 95 ℃ for 1min, rolling residual rate of 65 percent, and drying at 110 ℃ for 55 s. Transferring into a 3% polyester solution tank, soaking at 45 deg.C for 45s, and oven drying at 85 deg.C for 7min to obtain outer layer yarn.
The yarn is loaded into the front needle bed of the warp knitting machine to form a warp flat structure, and the rear needle bed of the rare earth-based heat transfer yarn is loaded into the warp knitting machine to form a six-hole mesh structure. The warp knitting layers woven by the front needle bed and the back needle bed are connected with the heat-transfer warm-keeping layer by driving yarns through the yarn guide comb. The density of the warp knitting yarns of the heating layer is 5 times of that of the heat transfer warm-keeping layer.
The fabrics prepared in examples 6-9 and comparative examples 1-4 were subjected to infrared irradiation temperature rise test, and the temperature difference was measured with reference to the fabric which was not impregnated with the rare earth-based infrared temperature rise impregnation solution in comparative example 4, and the results are shown in the following table:
TABLE 1 Infrared irradiation temperature rise test results
Fabric sample Temperature difference (. degree. C.)
Example 6 2.4
Example 7 3.9
Example 8 5.3
Example 9 4.8
Comparative example 1 1.7
Comparative example 2 1.9
Comparative example 3 1.5
Comparative example 4 0.6
The data results in the above table show that, because the structural density of the heat transfer warm-keeping layer is dense outside and sparse inside, the heat transfer connecting line is tight outside and loose inside, the internal temperature is reduced, the heat flux is transferred to the heating layer, meanwhile, the rare earth-based heat transfer material is lacked, the heat transfer yarn has excellent heat conduction performance, and the heat energy self-heating layer has low inward transfer efficiency. In the solar spectrum, lanthanum hexaboride mainly absorbs 780-1300nm near infrared rays; lanthanum cerium hexaboride mainly absorbs near infrared rays of 800-; samarium hexaboride, europium hexaboride, gadolinium hexaboride and yttrium hexaboride mainly absorb near infrared rays of 800-1500 nm. TTO mainly absorbs near infrared rays of 900-. Therefore, the rare earth hexaboride and the TTO material play a role in near infrared synergistic absorption on the near infrared spectrum, and the near infrared absorption defect is made up.
The fabrics prepared in example 6 and comparative examples 2 and 4 were subjected to accelerated aging test, and infrared heating fabric was subjected to 1.5KW/m2Ultraviolet (280-400 nm) accelerated aging test, wherein the radiation dose is the ultraviolet dose (5W/m) of a common solar light source2) 300 times. The test results are given in the following table:
TABLE 2 accelerated aging test results
Sample (I) Accelerated aging time Infrared absorption rate before aging Infrared absorption rate after aging
Comparative example 4 240h 0 0
Example 6 240h 99% 75%
Comparative example 2 240h 95% 23%
From the test results in the table above, it can be concluded that the W atom of the TTO material has photocatalytic properties, so that the infrared absorption performance of the TTO material decreases more and more rapidly, because the W atom of the radical continuously catalyzes the hexagonal structure WO3Leading to the increase of the W atom of the free radical, and the increased W atom of the free radical continuously catalyzes the hexagonal structure WO3Therefore, the infrared absorption property is more rapidly degraded. The cubic crystal hexaboride is ineffective due to oxidation and ultraviolet aging of a coated polymer dispersant, so that the infrared absorption performance is linearly reduced. The rare earth hexaboride is combined with TTO, so that the ageing resistance is enhanced in comprehensive performance at 150-450 h.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, so that any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present invention, should be included in the scope of the present invention.

Claims (9)

1. A rare earth-based infrared heating warm-keeping fabric is characterized in that: the yarn-impregnated rare earth-based infrared heating yarn is prepared by impregnating yarn with rare earth-based infrared heating impregnation liquid, the heat transfer and warm-keeping layer is prepared by impregnating yarn with rare earth-based heat transfer yarn which is prepared by impregnating yarn with rare earth-based high-heat-transfer impregnation liquid;
the rare earth-based infrared heating impregnation liquid contains 0.1-30 wt% of rare earth-based infrared heating slurry, and the rare earth-based infrared heating slurry comprises the following weightThe weight portions of the raw materials are as follows: 10-30 parts of near-infrared absorption powder, 45-99 parts of dispersion medium A and 1-15 parts of dispersing agent A, wherein the near-infrared absorption powder comprises 16-60 parts by weight of rare earth hexaboride and 40-84 parts by weight of cesium tungsten bronze, the rare earth hexaboride comprises 5-20 parts by weight of lanthanum hexaboride and 5-10 parts by weight of CexLa1-xB61-10 parts by weight of SmxLa1-xB65-10 parts by weight of EuxLa1-xB60-5 parts by weight of GdxLa1-xB60 to 5 parts by weight of YxLa1-xB6Wherein X takes a value of 0.1-0.9;
the rare earth-based high heat transfer impregnating solution contains 0.1-60 wt% of rare earth-based high heat transfer slurry, and the rare earth-based high heat transfer slurry comprises the following raw materials in parts by weight: 30-60 parts of heat transfer powder, 45-99 parts of dispersion medium B and 10-25 parts of dispersing agent B, wherein the heat transfer powder comprises 1-15 parts of yttrium zirconium oxide, 10-30 parts of lanthanum cerium oxide, 10-30 parts of lanthanum samarium oxide, 20-40 parts of silicon carbide and 20-40 parts of carbon black composite graphene.
2. The rare earth-based infrared heating and warming fabric according to claim 1, characterized in that: the particle size distribution of the near infrared absorption powder is 50-130nm, and the particle size distribution of the heat transfer powder is 200-450 nm.
3. The rare earth-based infrared heating and warming fabric according to claim 1, characterized in that: the dispersion medium A and the dispersion medium B are respectively and independently selected from one or more of deionized water, ethanol, ethylene glycol, propylene glycol methyl ether acetate, ethylene glycol butyl ether acetate, polymethyl methacrylate, dimethyl succinate, dimethyl glutarate and ethyl acetate.
4. The rare earth-based infrared heating and warming fabric according to claim 1, characterized in that: the dispersant A and the dispersant B are respectively and independently selected from one or more of sodium hexametaphosphate, sodium tripolyphosphate, sodium benzene sulfonate, azabenzene pyridine, alkyne diol, polyamide wax, polyolefin wax, polycarbodiimide, hydrogenated lecithin, N-methyl pyrrolidone solution of modified polyurea and cymene diol.
5. The rare earth-based infrared heating and warming fabric according to claim 1, characterized in that: the heating layer and the heat transfer warm-keeping layer are independently selected from single-sided fabric, double-sided fabric or spacer fabric; the yarn materials of the heating layer and the heat transfer warm-keeping layer are respectively selected from cotton fabrics, linen fabrics, wool fabrics, silk fabrics and chemical fibers.
6. The rare earth-based infrared heating and warming fabric according to claim 1, characterized in that: the yarn density of the heating layer is 5-10 times of that of the heat transfer warm-keeping layer.
7. A preparation method of the rare earth-based infrared heating and warm-keeping fabric disclosed by claims 1-6 is characterized in that: the preparation method of the rare earth-based infrared heating yarn comprises the following steps:
the method comprises the following steps: uniformly mixing 0.1-30 wt% of rare earth-based infrared heating material slurry, 1-10 wt% of adhesive and 1-5 wt% of flatting and softening agent in a high-speed dispersion machine, and injecting the mixture into an impregnation tank;
step two: soaping the yarn in 35-45 ℃ water bath for 5-12min, dehydrating and drying at 80-85 ℃ for 3-7 min;
step three: cleaning, and then conveying the mixture into a dipping tank for dipping at the pH of 7.5-8.5, wherein the dipping temperature is 65-75 ℃, the dipping time is 5-7min, and the rolling residue rate is 75-85%;
step four: secondary impregnation, wherein the impregnation temperature is 95-99 ℃, the impregnation time is 1-3min, the rolling residue rate is 65-75%, the drying temperature is 90-120 ℃, and the drying time is 55-75 s;
step five: transferring the mixture into a 3-7% polyester solution pool, soaking the mixture for 45-65s at the temperature of 35-55 ℃ in the pool, and drying the mixture for 3-7min at the temperature of 80-85 ℃ to obtain the rare earth-based infrared heating yarn.
8. A preparation method of the rare earth-based infrared heating and warm-keeping fabric disclosed by claims 1-6 is characterized in that: the preparation method of the rare earth-based heat transfer yarn comprises the following steps:
the method comprises the following steps: uniformly mixing 0.1-60 wt% of rare earth-based high-heat-transfer slurry, 1-10 wt% of adhesive and 1-5 wt% of flatting agent in a high-speed dispersion machine, and injecting the mixture into a dipping tank;
step two: soaping the yarn in 35-45 ℃ water bath for 5-12min, dehydrating and drying at 80-85 ℃ for 3-7 min;
step three: cleaning, and then conveying the mixture into a dipping pool for dipping at the pH value of 7.5-8.5 and the dipping temperature of 65-75 ℃, wherein the dipping time is 5-7min, and the rolling allowance rate is 75-85%;
step four: secondary impregnation, wherein the impregnation temperature is 95-99 ℃, the impregnation time is 1-3min, the rolling residue rate is 65-75%, the drying temperature is 90-120 ℃, and the drying time is 55-75 s;
step five: transferring the mixture into a 3-7% polyester solution pool, soaking the mixture for 45-65s at the temperature of 35-55 ℃ in the pool, and drying the mixture for 3-7min at the temperature of 80-85 ℃ to obtain the rare earth-based heat transfer yarn.
9. Use of the rare earth based infrared heating and warming fabric according to any one of claims 1 to 6 in the fields of clothing and home textiles.
CN202210436412.4A 2022-04-25 2022-04-25 Rare earth-based infrared heating and warming fabric and preparation method and application thereof Active CN114541138B (en)

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CN117385498A (en) * 2023-12-07 2024-01-12 天津包钢稀土研究院有限责任公司 Rare earth-based high-emissivity thermal physiotherapy composite fiber and preparation method thereof

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CN105544205A (en) * 2015-12-30 2016-05-04 江阴市长泾花园毛纺织有限公司 Breathable and warm air layer fabric
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CN1379075A (en) * 2001-04-06 2002-11-13 王庆波 Warming function material
CN1414168A (en) * 2001-10-26 2003-04-30 青岛大学 Bactericidal and for infrared radiation fabric or fibre and its preparation method
CN1989278A (en) * 2004-07-15 2007-06-27 住友金属矿山株式会社 Fiber containing boride microparticle and textile product therefrom
CN105544205A (en) * 2015-12-30 2016-05-04 江阴市长泾花园毛纺织有限公司 Breathable and warm air layer fabric
CN107513293A (en) * 2017-08-10 2017-12-26 广州市黑本新材料科技有限公司 A kind of preparation method of caesium tungsten bronze modified powder and its slurry

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117385498A (en) * 2023-12-07 2024-01-12 天津包钢稀土研究院有限责任公司 Rare earth-based high-emissivity thermal physiotherapy composite fiber and preparation method thereof

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