Elastic fiber capable of shielding near infrared rays as well as preparation method and application of elastic fiber
By using styrene-ethylene-butene-styrene block copolymer to prepare elastic fibers, and adding components such as MXene for impregnation during the preparation process, the problem of taking into account the mechanical properties and near-infrared shielding effect of elastic fibers is solved, and efficient near-infrared shielding and excellent mechanical properties are achieved.
Patent Information
- Application Number
- CN202311565675.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-22
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2043-11-22
AI Technical Summary
The existing elastic fibers are difficult to take into account both the mechanical properties and the near-infrared shielding effect, and cannot have excellent mechanical properties and effective near-infrared shielding ability at the same time.
Elastic fibers are prepared by using styrene-ethylene-butene-styrene block copolymer as raw material, and the near-infrared shielding effect of the fiber is improved by impregnating the impregnation solution composed of MXene, dopamine hydrochloride and dispersant in the presence of a solvent.
The prepared near-infrared shieldable elastic fibers not only have excellent near-infrared shielding effect, but also maintain good mechanical properties, and have simple process and economic value and application prospects.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fiber processing, and in particular to an elastic fiber capable of near-infrared shielding, a preparation method and application thereof. Background Art
[0002] Infrared stealth technology is to reduce the detectability of a target by reducing or changing its infrared radiation characteristics. It mainly includes changing the infrared radiation characteristics of the target, reducing the infrared radiation intensity of the target, and adjusting the propagation path of infrared radiation. Specific measures include improving thermal structure design, forcibly cooling the main heating components, coating the surface with infrared stealth materials, and using infrared camouflage and shielding. The purpose of infrared stealth is to reduce or change the infrared radiation characteristics of the target, reduce the range of the infrared detection system to the target, and thus reduce the probability of the target being detected.
[0003] Infrared stealth materials mainly include infrared low-emissivity stealth materials, cooling camouflage coatings, etc. For example, metal plating is to electrochemically oxidize various metals or alloys, such as aluminum, copper, iron, etc., to form a thin and dense oxide film, thereby reflecting radiation; the second is ceramic coating, that is, using inorganic non-metallic materials as coatings to cover the entire surface with a uniform and solid ceramic layer, thereby reflecting rays; the third is fiber weaving, that is, using natural or synthetic high-molecular organic compounds, interwoven with fibers after special processing, to make fabrics of different structures.
[0004] However, although the first two methods mentioned above have good infrared stealth capabilities, due to the large specific gravity of the materials, they are generally used for infrared stealth of large devices and are not suitable for small items such as clothing. The special processing using natural or synthetic high-molecular organic compounds is often more complicated and has a poor near-infrared shielding effect.
[0005] CN109869646A discloses a method for preparing electromagnetic shielding fabric based on two-dimensional layered MXene nanosheets, which is characterized by comprising the following steps: (1) pre-treating the fabric with sodium hydroxide and sodium carbonate aqueous solution to remove oil stains and impurities on the surface of the fabric, washing with distilled water and drying; (2) weighing a certain amount of MAX phase Ti 3 AlC 2, soaked in a 10%-50% hydrofluoric acid aqueous solution, stirred for 18-24h, then filtered and washed with distilled water, and dried to obtain MXene powder; (3) MXene powder was dissolved in a certain amount of water, and a certain concentration of MXene solution was obtained by ultrasonic treatment; (4) MXene solution was first sprayed on one side of the pretreated fabric and dried, and then MXene solution was sprayed on the other side of the fabric and dried. The MXene solution spraying process was uniform to obtain MXene modified fabric. This scheme adopts the spraying method, which is not conducive to large-scale preparation, and spraying can only perform surface modification. For fibers with complex internal network structures, good modification cannot be achieved inside, and the near-infrared shielding ability is lost when the surface is worn or damaged. Summary of the invention
[0006] The purpose of the present invention is to solve the problem that the mechanical properties and near infrared shielding effect of elastic fibers in the prior art cannot be taken into account at the same time.
[0007] In order to achieve the above object, the first aspect of the present invention provides a method for preparing an elastic fiber capable of near infrared shielding, the method comprising:
[0008] (1) drying and melt-spinning a styrene-ethylene-butylene-styrene block copolymer in sequence to obtain an elastic fiber; and
[0009] In the presence of a solvent, MXene, dopamine hydrochloride and a dispersant are mixed to obtain an impregnation solution;
[0010] (2) immersing the elastic fiber in an immersion liquid to obtain the elastic fiber capable of near infrared shielding;
[0011] The solvent is a mixed solution of water and dimethylformamide in a volume ratio of 1:1-1.5;
[0012] Relative to every 100 mL of solvent, the amount of MXene used is 0.16-0.45 g, the amount of dispersant used is 0.3-0.75 g, and the amount of dopamine hydrochloride used is 0.008-0.012 mol;
[0013] The dispersant is selected from at least one of sodium hexametaphosphate, sodium tripolyphosphate and sodium humate.
[0014] The second aspect of the present invention provides an elastic fiber capable of near infrared shielding prepared by the method described in the first aspect.
[0015] The third aspect of the present invention provides application of the near-infrared shielding elastic fiber described in the second aspect in the textile field.
[0016] The present invention adopts styrene-ethylene-butylene-styrene block copolymer as raw material to prepare elastic fiber, and performs impregnation treatment through a specific impregnation liquid. The prepared elastic fiber capable of near-infrared shielding has excellent near-infrared shielding effect and mechanical properties. The preparation method provided by the present invention has a simple process and has good economic value and application prospects. DETAILED DESCRIPTION
[0017] The endpoints and any values of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, the endpoint values of each range and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.
[0018] As mentioned above, the first aspect of the present invention provides a method for preparing an elastic fiber capable of near infrared shielding, the method comprising:
[0019] (1) drying and melt-spinning a styrene-ethylene-butylene-styrene block copolymer in sequence to obtain an elastic fiber; and
[0020] In the presence of a solvent, MXene, dopamine hydrochloride and a dispersant are mixed to obtain an impregnation solution;
[0021] (2) immersing the elastic fiber in an immersion liquid to obtain the elastic fiber capable of near infrared shielding;
[0022] The solvent is a mixed solution of water and dimethylformamide in a volume ratio of 1:1-1.5;
[0023] Relative to every 100 mL of solvent, the amount of MXene used is 0.16-0.45 g, the amount of dispersant used is 0.3-0.75 g, and the amount of dopamine hydrochloride used is 0.008-0.012 mol;
[0024] The dispersant is selected from at least one of sodium hexametaphosphate, sodium tripolyphosphate and sodium humate.
[0025] Preferably, the preparation steps of the MXene include:
[0026] S1, mixing lithium fluoride and hydrochloric acid for the first time to obtain a mixed solution;
[0027] S2. Under stirring, mixing aluminum titanium carbide with the mixed solution for a second time to obtain a solution containing MXene;
[0028] S3, washing the MXene-containing solution with water and centrifuging it in sequence to obtain a precipitate;
[0029] S4. freeze-drying the precipitate to obtain the MXene.
[0030] Preferably, for every 1 g of lithium fluoride, the amount of hydrochloric acid used is 15-30 mL, and the amount of aluminum carbotitanium used is 0.8-1.2 g.
[0031] It should be noted that in the present invention, in the step of preparing MXene, there is no special requirement for the first mixing condition, as long as the lithium fluoride can be completely dissolved. The present invention will not be elaborated here, and those skilled in the art should not understand it as a limitation of the present invention.
[0032] Preferably, the second mixing conditions are: temperature of 30-35° C., and time of 22-26 h.
[0033] Preferably, before performing step (2), the elastic fiber is cleaned in acetone, anhydrous ethanol and water respectively in sequence, and the ultrasonic cleaning time is 4-8 minutes.
[0034] Preferably, the amount of MXene used is 0.2-0.3 g per 100 mL of solvent. The inventors found that under this preferred embodiment, the elastic fiber obtained by the present invention has a more excellent near-infrared shielding effect and better mechanical properties.
[0035] Preferably, the amount of the dispersant used is 0.4-0.5 g per 100 mL of solvent.
[0036] Preferably, the amount of dopamine hydrochloride used is 0.008-0.01 mol relative to 100 mL of solvent.
[0037] Preferably, the dispersant is sodium hexametaphosphate. The inventors found that under this preferred embodiment, the elastic fiber obtained by the present invention has a more excellent near-infrared shielding effect and better mechanical properties.
[0038] Preferably, the content of styrene structural units of the styrene-ethylene-butylene-styrene block copolymer is 15-30wt%, the Shore A hardness is 50-60, the melt index (230°C, 2.16Kg) is 210-220g / min or the melt index (200°C, 5Kg) is 25-35g / min. The inventors found that under this preferred embodiment, the elastic fiber obtained by the present invention has a more excellent near-infrared shielding effect and better mechanical properties.
[0039] Preferably, in step (1), the melt spinning step comprises: melt extrusion, melt extrusion, receiving and winding; the temperature of the melt extrusion and melt extrusion is 160-175°C.
[0040] More preferably, the melt spinning step further comprises: filtering and metering in sequence before melt extrusion; the filtering and metering temperatures are both 160-175°C.
[0041] It should be noted that, in the present invention, each step of the melt spinning is carried out by a conventional method in the art, which will not be described in detail herein, and those skilled in the art should not interpret this as a limitation to the present invention.
[0042] Preferably, the receiving and winding temperatures are both 90-100°C, and the winding speed is 50-200rpm. It should be noted that in the present invention, the temperatures of different areas of the melt spinning machine are different, and the speeds of different rollers during the winding process are also different, so the conditions of the melt spinning are all achieved within the aforementioned range. The present invention will not be repeated here, and those skilled in the art should not be understood as limiting the present invention.
[0043] Preferably, in step (2), the immersion treatment is carried out under ultrasonic conditions, and the conditions of the immersion treatment include: a temperature of 25-30° C. and a time of 30-90 min.
[0044] As mentioned above, the second aspect of the present invention provides an elastic fiber capable of near infrared shielding prepared by the method described in the first aspect.
[0045] As mentioned above, the third aspect of the present invention provides the use of the near-infrared shielding elastic fiber described in the second aspect in the textile field.
[0046] The present invention will be described in detail below through examples.
[0047] In the following examples, unless otherwise specified, the experimental instruments, reagents and raw materials involved are all commercially available, and the reagents are all analytically pure products.
[0048] Styrene-ethylene-butylene-styrene block copolymer: model MD-1648, the content of styrene structural unit is 20wt%, Shore A hardness is 52, and the melt index (230℃, 2.16Kg) is 220g / min, purchased from Kraton, USA; model YH-505, the content of styrene structural unit is 20wt%, Shore A hardness is 56, and the melt index (200℃, 5Kg) is 30g / min, purchased from Sinopec Baling Petrochemical Company; model YH-602, the content of styrene structural unit is 35wt%, Shore A hardness is 80, purchased from Sinopec Baling Petrochemical Company.
[0049] Preparation Example 1
[0050] This preparation example is used to illustrate that MXene in the present invention is prepared according to the following steps.
[0051] S1. Firstly mix 1 g of lithium fluoride with 20 ml of 9 mol / L hydrochloric acid to obtain a mixed solution;
[0052] S2. Under stirring (stirring speed is 200 rpm), 1 g of aluminum titanium carbide is mixed with the mixed solution for a second time (temperature is 35° C., time is 24 h) to obtain a solution containing MXene;
[0053] S3, washing the MXene-containing solution with water and centrifuging it in sequence (the centrifugal speed is 3500 rpm) to obtain a precipitate;
[0054] S4. freeze-drying the precipitate to obtain the MXene.
[0055] Example 1
[0056] This example is used to illustrate that the elastic fiber capable of near-infrared shielding of the present invention is prepared according to the formula and process parameters in Table 1 and the method described below.
[0057] Step 1: drying, melt-extruding, filtering, metering, melt-extruding, receiving and winding the styrene-ethylene-butylene-styrene block copolymer to obtain elastic fibers; and mixing MXene, dopamine hydrochloride and a dispersant in the presence of a solvent to obtain an impregnation solution;
[0058] The drying conditions are: temperature 40°C, time 6 hours;
[0059] The temperature of melt extrusion, filtration, metering and melt extrusion is 160-175°C, the temperature of receiving and winding is 90-100°C, and the speed of winding is 50-200rpm;
[0060] Step 2: ultrasonically cleaning the elastic fiber in acetone for 5 minutes, ultrasonically cleaning in anhydrous ethanol for 5 minutes, and ultrasonically cleaning in deionized water for 5 minutes;
[0061] Step three: immersing the elastic fiber after ultrasonic cleaning in the immersion liquid to obtain the elastic fiber capable of near-infrared shielding.
[0062] Unless otherwise specified, the remaining examples were carried out using a process similar to that of Example 1, except that the formulations and process parameters used in each example were different, see Table 1 for details (Note: the parameters not listed in Table 1 are the same as the corresponding parameters in Example 1).
[0063] Table 1
[0064]
[0065] Comparative Example 1
[0066] This comparative example was carried out using a process similar to that of Example 1, except that no dispersant was used in this comparative example.
[0067] The rest are the same as in Example 1.
[0068] The elastic fiber DS1 capable of near-infrared shielding was prepared.
[0069] Comparative Example 2
[0070] This comparative example was carried out using a process similar to that of Example 1, except that the amount of MXene used in this comparative example was 0.1 g.
[0071] The rest are the same as in Example 1.
[0072] The elastic fiber DS2 capable of near infrared shielding was prepared.
[0073] Comparative Example 3
[0074] This comparative example was carried out using a process similar to that of Example 1, except that the amount of MXene used in this comparative example was 0.5 g.
[0075] The rest are the same as in Example 1.
[0076] The elastic fiber DS3 capable of near infrared shielding was prepared.
[0077] Comparative Example 4
[0078] This comparative example was carried out using a process similar to that of Example 1, except that the amount of the dispersant used in this comparative example was 0.8 g.
[0079] The rest are the same as in Example 1.
[0080] The elastic fiber DS4 capable of near-infrared shielding was prepared.
[0081] Comparative Example 5
[0082] This comparative example is carried out using a process similar to that of Example 1, except that an equal mass of lignin (model P-d3, manufactured by Shanghai Aladdin Biochemical Technology Co., Ltd.) is used in this comparative example to replace the sodium hexametaphosphate in Example 1.
[0083] The rest are the same as in Example 1.
[0084] The elastic fiber DS5 capable of near infrared shielding was prepared.
[0085] Test Case
[0086] The same method was used to test the performance of the near infrared shielding elastic fibers prepared in the embodiment and the comparative example, and the results are shown in Table 2.
[0087] 1. The tensile strength and elongation at break of the elastic fiber were measured by a universal material mechanical properties tester (model UTM4104, manufacturer Shenzhen Sansi Zongheng Technology Co., Ltd.);
[0088] 2. Use a near-infrared camera to observe the surface temperature of the elastic fiber at 50°C for 600 seconds. The lower the surface temperature, the stronger the near-infrared shielding ability.
[0089] 3. Use a universal material mechanical properties tester (model UTM4104, manufacturer Shenzhen Sansi Zongheng Technology Co., Ltd.) to stretch the sample at a length of 5 cm and a stretching speed of 500 mm / min. The stretching length is 200%, and then the sample is recovered at a speed of 500 mm / min.
[0090] Table 2
[0091] project Tensile strength / MPa Elongation at break Surface observation temperature / ℃ Elastic recovery rate % Example 1 15.2 345.24% 30.1 96 Example 2 14.7 338.42% 31.8 97 Example 3 16.3 289.45% 29.5 95 Example 4 14.5 330.11% 32.3 95 Example 5 14.4 326.53% 31.7 92 Example 6 18.3 280.66% 32.2 93 Comparative Example 1 11.6 316.76% 42.5 92 Comparative Example 2 11.4 298.54% 43.3 89 Comparative Example 3 10.8 289.36% 39.8 85 Comparative Example 4 11.9 312.58% 41.5 91 Comparative Example 5 12.7 312.79% 36.7 80
[0092] It can be seen from the results in Table 2 that the elastic fiber obtained by the present invention has better near-infrared shielding effect and excellent mechanical properties.
[0093] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.
Claims
1. A method for preparing elastic fibers capable of near infrared shielding, It is characterized in that The method includes: (1) drying and melt-spinning a styrene-ethylene-butylene-styrene block copolymer in sequence to obtain an elastic fiber; and In the presence of a solvent, MXene, dopamine hydrochloride and a dispersant are mixed to obtain an impregnation solution; (2) immersing the elastic fiber in an immersion liquid to obtain the elastic fiber capable of near infrared shielding; The solvent is a mixed solution of water and dimethylformamide in a volume ratio of 1:1-1.5; Relative to every 100 mL of solvent, the amount of MXene used is 0.16-0.45 g, the amount of dispersant used is 0.3-0.75 g, and the amount of dopamine hydrochloride used is 0.008-0.012 mol; The dispersant is selected from at least one of sodium hexametaphosphate, sodium tripolyphosphate and sodium humate.
2. The method according to claim 1, It is characterized in that The amount of MXene used is 0.2-0.3 g per 100 mL of solvent.
3. The method according to claim 1 or 2, It is characterized in that The amount of the dispersant is 0.4-0.5 g per 100 mL of solvent; And / or, relative to 100 mL of the solvent, the amount of dopamine hydrochloride used is 0.008-0.01 mol.
4. The method according to any one of claims 1 to 3, It is characterized in that The dispersant is sodium hexametaphosphate.
5. The method according to any one of claims 1 to 4, It is characterized in that The styrene structural unit content of the styrene-ethylene-butylene-styrene block copolymer is 15-30wt%, the Shore A hardness is 50-60, the melt index at 230°C and 2.16Kg is 210-220g / min, or the melt index at 200°C and 5Kg is 25-35g / min.
6. The method according to any one of claims 1 to 5, It is characterized in that In step (1), the melt spinning steps include: melt extrusion, melt extrusion, receiving and winding; the temperatures of the melt extrusion and melt extrusion are both 160-175°C.
7. The method according to claim 6, It is characterized in that The receiving and winding temperatures are both 90-100° C., and the winding rotation speed is 50-200 rpm.
8. The method according to any one of claims 1 to 7, It is characterized in that In step (2), the immersion treatment is carried out under ultrasonic conditions, and the conditions of the immersion treatment include: temperature of 25-30° C. and time of 30-90 min.
9. Elastic fiber capable of near infrared shielding prepared by the method according to any one of claims 1 to 8.
10. Use of the near-infrared shielding elastic fiber according to claim 9 in the textile field.
Citation Information
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