Method for applying graphene to natural cotton textile material

By immersing the graphene oxide solution in cotton yarn and stacking, heating, reduction and other treatments, the problem that graphene and natural fiber composite technology has not yet been industrialized, and the preparation of functional graphene yarns is achieved, with excellent functionality and performance.

CN119800697APending Publication Date: 2025-04-11HEBEI UNIV OF SCI & TECH
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Patent Information

Application Number
CN202411979273.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-31
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

In the prior art, graphene is mainly used in chemical fiber substrates, and has not yet achieved effective composite with natural fibers, making it difficult to meet the multiple requirements of high-end people for functionality, originality and comfort.

Method used

By preparing graphene oxide solution, impregnating cotton yarns, and combining graphene with natural cotton textile materials through stacking, heating, reduction, soap washing and water washing and drying.

Benefits of technology

The obtained functional graphene yarn has the advantages of simple process, high composite efficiency, good washing fastness and good friction fastness, and imparts the yarn with antibacterial, deodorizing, antistatic, far-infrared health care, negative ion generation and ultraviolet protection.

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Abstract

The invention discloses a method for applying graphene to a natural cotton textile material. The method comprises the following steps: step 1, preparing a graphene oxide solution; step 2, dipping the cotton yarns; step 3, adding an auxiliary agent; 4, stacking the yarns; 5, yarn heating; step 6, reduction treatment; step 7, soaping treatment; step 8, washing and drying; graphene oxide and the yarn are compounded in a stacking mode, the graphene functional yarn is obtained after heating, reduction, soaping, water washing and drying treatment, the graphene functional yarn has the advantages of being simple in process, high in compounding efficiency, good in water washing fastness and good in rubbing fastness, the compounded yarn can keep original mechanical performance, fabrics of different styles can be flexibly designed, and the graphene functional yarn is suitable for being popularized and applied. Meanwhile, a functional fabric prepared from the functional graphene yarn has the functions of antibiosis, deodorization, static resistance, far infrared health care, negative ion generation and ultraviolet protection, and is beneficial to human health.
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Description

Technical Field

[0001] The invention relates to the technical field of functional textile materials, in particular to a method for applying graphene to natural cotton textile materials. Background Art

[0002] Since the discovery of graphene, many countries and regions around the world have carried out graphene-related research. At present, there are a large number of graphene companies, and there are also a certain number of graphene industrial parks, research institutes, innovation centers and industrial alliances. However, what follows is the reality of overcapacity of graphene. Although the graphene production capacity is high, the utilization rate is low. To change this situation, we must base ourselves on the manufacturing industry, make long-term plans, and accelerate the move towards the middle and high end of the industrial chain. Therefore, the research and development of core technologies on the application end is particularly important. Realizing the high added value of textile materials needed for national economy and people's livelihood is an effective path to transform effective carbon emissions and achieve low-carbon development. In the existing technology, the composite of graphene and textile materials is mainly the production of chemical fiber substrates such as polyester, acrylic, nylon and viscose. The composite technology of natural fibers has not yet been industrialized, which makes it difficult to meet the multiple requirements of high-end people for the functionality, original ecology and comfort of fiber materials. At the same time, the product design of downstream yarns, fabrics and finished products also needs to be expanded to high-end. Therefore, a method for applying graphene to natural cotton textile materials is proposed. Summary of the invention

[0003] The object of the present invention is to provide a method for applying graphene to natural cotton textile materials to solve the problems raised in the above background technology.

[0004] To achieve the above object, the present invention provides the following technical solution: a method for applying graphene to natural cotton textile materials, comprising the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0005] Step 1: preparing a graphene oxide solution with a concentration of 1-10% and a bath ratio of 1:5-50, and performing ultrasonic dispersion treatment on the graphene oxide solution;

[0006] Step 2: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1;

[0007] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution;

[0008] Step 4 is: taking out the yarn impregnated in step 3, stacking for 4-48 hours, repeating the impregnation and stacking steps 1-3 times, so that the amount of liquid in the yarn is controlled at 80-150%;

[0009] Step 5: taking out the yarn piled in step 4 and heating it at 65-160° C. for 3-50 minutes;

[0010] Step six is: taking out the yarn after the heating treatment in step five and immersing it in the reducing solution;

[0011] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing;

[0012] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0013] Preferably, in step 1, the lateral size of the graphene oxide is between 100 nm and 50 μm, and the number of layers is between 1 and 9.

[0014] Preferably, in step 1, the ultrasonic dispersion treatment time is 10-240 min.

[0015] Preferably, in step 2, the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn is impregnated for 1-30 minutes.

[0016] Preferably, in step three, the inorganic salt is one or more of nitrate, sulfate, phosphate, and chloride, and the concentration is 1-100 times the concentration of graphene. The dispersant is one or more of anionic dispersants and non-ionic dispersants, and the concentration is 0.01-10 g / L. The immersion time of the yarn is 1-30 min.

[0017] Preferably, in step six, the immersion temperature is 50-100° C., and the immersion time is 3-100 min.

[0018] Preferably, in step six, the reducing solution is prepared using 1-15 g / L of alkali agent and 1-15 g / L of reducing powder, with a bath ratio of 1:5-50.

[0019] Preferably, the alkali agent is one or more of hydroxide, phosphate, carbonate, sulfate, and ammonia-soluble alkali.

[0020] Preferably, the reducing powder is one or more of metal complexing agents, divalent sulfur compounds, sulfites, vitamins, and hydrazine compounds.

[0021] Preferably, in step seven, the bath ratio used in the soaping treatment is 1:5-50, the soap flake concentration is 1-20 g / L, the soaping temperature is 50-100° C., and the soaping time is 5-240 min.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows: the present invention uses a stacking method to compound graphene oxide with yarn, and obtains graphene functional yarn after heating, reduction, soaping, washing and drying. The present invention has the advantages of simple process, high compounding efficiency, good water washing fastness and good friction fastness. The yarn after compounding can maintain the original mechanical properties, and fabrics of different styles can be flexibly designed. At the same time, the functional fabric prepared by using the functional graphene yarn has the functions of antibacterial, deodorizing, antistatic, far-infrared health care, negative ion generation and ultraviolet protection, which is beneficial to human health. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 is a flow chart of the method of the present invention;

[0024] Figure 2 This is a real picture of the graphene functional yarn bobbin of the present invention;

[0025] Figure 3 This is a physical picture of the functional fabric of the present invention;

[0026] Figure 4 The K / S value variation trend of the graphene functional fabric of the present invention at different light wavelengths;

[0027] Figure 5 The thermogravimetric diagram of the untreated pure cotton yarn, graphene functional yarn and graphene finishing agent of the present invention;

[0028] Figure 6 The graphene treatment liquid of the present invention;

[0029] Figure 7 This is a diagram showing the stacking state of the yarn after being impregnated with the treatment liquid of the present invention. DETAILED DESCRIPTION

[0030] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] Please see attached Figure 1 -Attached Figure 7 , a technical solution provided by the present invention:

[0032] Embodiment 1:

[0033] A method for applying graphene to natural cotton textile materials comprises the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0034] Step 1: prepare a graphene oxide aqueous dispersion with a concentration of 3.3% and a bath ratio of 1:30, and perform ultrasonic dispersion treatment on the graphene oxide solution; wherein the lateral size of the graphene oxide is about 1 μm, and the number of layers is 1-3; and the ultrasonic dispersion treatment time is 30-60 minutes;

[0035] Step 2 is: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; wherein the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn immersion time is 10 minutes;

[0036] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; wherein the inorganic salt is one or two of sulfate, phosphate, and chloride, and the concentration is 10 times the concentration of graphene oxide, and the dispersant is a non-ionic dispersant, and the concentration is 1 g / L, and the immersion time of the yarn is 10 minutes;

[0037] Step 4 is: taking out the yarn impregnated in step 3, stacking it for 24 hours, squeezing out the water and then immersing it in the treatment solution of step 3 again for 10 minutes, stacking it for 24 hours, squeezing out the water so that the yarn liquid content is controlled at 120%;

[0038] Step 5: taking out the yarn piled in step 4 and heating it at 120° C. for 3 minutes;

[0039] Step six is: taking out the yarn after the heating treatment in step five, and immersing it in a reducing solution; wherein the immersion temperature is 60° C., the immersion time is 60 min, the reducing solution is prepared with 5 g / L of sodium hydroxide and 5 g / L of hydrosulfite, and the bath ratio is 1:40;

[0040] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing treatment; wherein the bath ratio used in the soap washing treatment is 1:40, the soap flake concentration is 2 g / L, the soap washing temperature is 90° C., and the soap washing time is 10 min;

[0041] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0042] The difference in color perception between the functional graphene yarn obtained after the above steps and the untreated yarn was measured using a computer automatic color matching system, represented by ΔE. The larger the value, the greater the color difference, which means that the adsorption of graphene on the yarn is greater. The ΔE obtained in this embodiment is 48.15. The graphene finishing agent and the weight of the yarn before and after the treatment are measured with the temperature using a thermogravimetric analyzer. The residual carbon content at 800°C is measured. The adsorption of graphene on the yarn is calculated to be 2.45% according to the following formula;

[0043]

[0044] Wherein, q is the adsorption amount of graphene on the yarn (%);

[0045] a is the residual carbon content of graphene functional yarn at 800 °C;

[0046] b is the residual carbon content of graphene finishing agent at 800 °C;

[0047] c is the residual carbon content of pure cotton yarn at 800°C;

[0048] It can be seen that this method can successfully compound graphene into pure cotton yarn. At the same time, the breaking strength and breaking elongation of the graphene functional yarn were measured to characterize its usability in subsequent weaving, as shown in Table 2. Combined with the above analysis, it can be seen that this method can prepare weavable functional yarns with a certain amount of graphene adsorption. The composite fastness of graphene in the yarn will be explained in the subsequent knitted fabric section.

[0049] Embodiment 2:

[0050] A method for applying graphene to natural cotton textile materials comprises the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0051] Step 1: prepare a graphene oxide aqueous dispersion with a concentration of 3.3% and a bath ratio of 1:30, and perform ultrasonic dispersion treatment on the graphene oxide solution; wherein the lateral size of the graphene oxide is about 1 μm, and the number of layers is 5-8; and the ultrasonic dispersion treatment time is 60 minutes;

[0052] Step 2 is: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; wherein the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn immersion time is 10 minutes;

[0053] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; wherein the inorganic salt is one or two of sulfate, phosphate, and chloride, and the concentration is 10 times the concentration of graphene oxide, the dispersant is a non-ionic dispersant, and the concentration is 3g / L, and the immersion time of the yarn is 10min;

[0054] Step 4 is: taking out the yarn impregnated in step 3, stacking it for 24 hours, squeezing out the water and then immersing it in the treatment solution of step 3 again for 10 minutes, stacking it for 24 hours, squeezing out the water so that the yarn liquid content is controlled at 120%;

[0055] Step 5: taking out the yarn piled in step 4 and heating it at 120° C. for 3 minutes;

[0056] Step six is: taking out the yarn after the heating treatment in step five, and immersing it in a reducing solution; wherein the immersion temperature is 60° C., the immersion time is 60 min, the reducing solution is prepared with 5 g / L of sodium hydroxide and 5 g / L of hydrosulfite, and the bath ratio is 1:40;

[0057] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing treatment; wherein the bath ratio used in the soap washing treatment is 1:40, the soap flake concentration is 2 g / L, the soap washing temperature is 90° C., and the soap washing time is 10 min;

[0058] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0059] The difference in color perception between the functional graphene yarn obtained after the above-mentioned treatment steps and the untreated yarn was determined using a computer automatic color matching system. The ΔE obtained in this embodiment was 32, and the adsorption of graphene on the yarn was measured and calculated using a thermogravimetric analyzer to be 1.58%. Compared with Example 1, Example 2 selected graphene with a larger number of layers. Although the ultrasonic time was slightly prolonged, a smaller adsorption amount was obtained under the same conditions of all other process conditions. It was found during the experiment that the floating color in the reduction step and the soaping step was more obvious than that in Example 1, indicating that the fewer the number of graphene layers and the smaller the size, the greater the accessibility in the fiber.

[0060] Embodiment 3:

[0061] A method for applying graphene to natural cotton textile materials comprises the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0062] Step 1: prepare a graphene oxide aqueous dispersion with a concentration of 3.3% and a bath ratio of 1:30, and perform ultrasonic dispersion treatment on the graphene oxide solution; wherein the lateral size of the graphene oxide is about 1 μm, and the number of layers is 1-3; and the ultrasonic dispersion treatment time is 20 minutes;

[0063] Step 2 is: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; wherein the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn immersion time is 10 minutes;

[0064] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; wherein the inorganic salt is one or two of sulfate, phosphate, and chloride, and the concentration is 10 times the concentration of graphene oxide, and the dispersant is a non-ionic dispersant, and the concentration is 2 g / L, and the immersion time of the yarn is 10 minutes;

[0065] Step 4: take out the yarn soaked in step 3, pile it for 24 hours, and squeeze out the water so that the amount of liquid in the yarn is controlled at 120%;

[0066] Step 5: taking out the yarn piled in step 4 and heating it at 120° C. for 3 minutes;

[0067] Step six is: taking out the yarn after the heating treatment in step five, and immersing it in a reducing solution; wherein the immersion temperature is 60° C., the immersion time is 60 min, the reducing solution is prepared with 5 g / L of sodium hydroxide and 5 g / L of hydrosulfite, and the bath ratio is 1:40;

[0068] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing treatment; wherein the bath ratio used in the soap washing treatment is 1:40, the soap flake concentration is 2 g / L, the soap washing temperature is 90° C., and the soap washing time is 10 min;

[0069] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0070] The difference in color perception between the functional graphene yarn obtained after the above-mentioned steps and the untreated yarn was determined using a computer automatic color matching system. The ΔE obtained in this embodiment was 40, and the adsorption of graphene on the yarn was measured and calculated using a thermogravimetric analyzer to be 1.98%. Compared with Example 1, step 4 of Example 3 was not treated with dipping again after stacking, so a smaller adsorption amount was obtained, but the reduction in the adsorption amount was less than half, indicating that increasing the number of dipping times can increase the adsorption amount to a certain extent, but it is not a linear relationship. In production practice, production costs and product quality should be considered in a coordinated manner.

[0071] Embodiment 4:

[0072] A method for applying graphene to natural cotton textile materials comprises the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0073] Step 1: prepare a graphene oxide aqueous dispersion with a concentration of 3.3% and a bath ratio of 1:30, and perform ultrasonic dispersion treatment on the graphene oxide solution; wherein the lateral size of the graphene oxide is about 1 μm, and the number of layers is 1-3; and the ultrasonic dispersion treatment time is 30-60 minutes;

[0074] Step 2 is: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; wherein the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn immersion time is 10 minutes;

[0075] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; wherein the inorganic salt is one or two of sulfate, phosphate, and chloride, and the concentration is 10 times the concentration of graphene oxide, and the dispersant is a non-ionic dispersant, and the concentration is 1 g / L, and the immersion time of the yarn is 10 minutes;

[0076] Step 4 is: taking out the yarn impregnated in step 3, stacking it for 24 hours, squeezing out the water and then immersing it in the treatment solution of step 3 again for 10 minutes, stacking it for 24 hours, squeezing out the water so that the yarn liquid content is controlled at 120%;

[0077] Step 5: taking out the yarn piled in step 4 and heating it at 120° C. for 3 minutes;

[0078] Step six is: taking out the yarn after the heating treatment in step five, and immersing it in a reducing solution; wherein the immersion temperature is 30° C., the immersion time is 30 min, the reducing solution is prepared with 5 g / L sodium hydroxide and 5 g / L hydrosulfite, and the bath ratio is 1:40;

[0079] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing treatment; wherein the bath ratio used in the soap washing treatment is 1:40, the soap flake concentration is 2 g / L, the soap washing temperature is 90° C., and the soap washing time is 10 min;

[0080] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0081] The difference in color perception between the functional graphene yarn obtained after the above-mentioned treatment steps and the untreated yarn was determined using a computer automatic color matching system. The ΔE obtained in this embodiment was 37.8, and the adsorption amount of graphene on the yarn was measured and calculated using a thermogravimetric analyzer to be 1.71%. Compared with Example 1, the reduction step of Example 4 was carried out at a lower temperature and in a shorter time, and a smaller adsorption amount was obtained. During the experiment, it was found that more floating color appeared in the soap washing step. It is speculated that the reason is that the reduction conditions are insufficient, and the graphene oxide on the yarn cannot be completely reduced. In the subsequent soap washing process, the graphene oxide is desorbed again.

[0082] Embodiment 5:

[0083] A method for applying graphene to natural cotton textile materials comprises the following steps: step 1, preparing a graphene oxide solution; step 2, impregnating cotton yarn; step 3, adding an auxiliary agent; step 4, stacking the yarn; step 5, heating the yarn; step 6, reducing treatment; step 7, soaping treatment; step 8, washing and drying;

[0084] Step 1: prepare a graphene oxide aqueous dispersion with a concentration of 3.3% and a bath ratio of 1:30, and perform ultrasonic dispersion treatment on the graphene oxide solution; wherein the lateral size of the graphene oxide is about 1 μm, and the number of layers is 1-3; and the ultrasonic dispersion treatment time is 30-60 minutes;

[0085] Step 2 is: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; wherein the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn immersion time is 10 minutes;

[0086] Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; wherein the inorganic salt is one or two of sulfate, phosphate, and chloride, and the concentration is 10 times the concentration of graphene oxide, and the dispersant is a non-ionic dispersant, and the concentration is 1 g / L, and the immersion time of the yarn is 10 minutes;

[0087] Step 4 is: taking out the yarn impregnated in step 3, stacking it for 24 hours, squeezing out the water and then immersing it in the treatment solution of step 3 again for 10 minutes, stacking it for 24 hours, squeezing out the water so that the yarn liquid content is controlled at 120%;

[0088] Step 5: taking out the yarn piled in step 4 and heating it at 120° C. for 3 minutes;

[0089] Step six is: taking out the yarn after the heating treatment in step five, and immersing it in the reducing solution; wherein the immersion temperature is 60° C., the immersion time is 60 min, the reducing solution is prepared with 5 g / L of hydrosulfite, and the bath ratio is 1:40;

[0090] Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing treatment; wherein the bath ratio used in the soap washing treatment is 1:40, the soap flake concentration is 2 g / L, the soap washing temperature is 90° C., and the soap washing time is 10 min;

[0091] Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

[0092] The difference in color perception between the functional graphene yarn obtained after the above-mentioned treatment steps and the untreated yarn was determined using a computer automatic color matching system. The ΔE obtained in this embodiment was 38.6. The adsorption amount of graphene on the yarn was measured and calculated using a thermogravimetric analyzer to be 1.68%. Compared with Example 1, the reduction step of Example 5 was carried out under neutral conditions, and a smaller adsorption amount was obtained. During the experiment, it was found that more floating color appeared in the soap washing step. It is speculated that the reason is that the insurance powder has a higher reduction activity under alkaline conditions, and the graphene oxide on the yarn cannot be completely reduced under neutral conditions. In the subsequent soap washing process, the graphene oxide is desorbed again.

[0093] Experimental Example 1:

[0094] The functional graphene yarn obtained in the above embodiment 1 is used to prepare a functional knitted fabric, specifically: the functional graphene yarn is subjected to a yarn splitting operation, the functional graphene yarn after the yarn splitting is subjected to a bobbin winding operation, and the functional graphene yarn bobbin is subjected to a knitting operation to obtain a functional knitted fabric; the composite fastness of graphene and yarn in the fabric is determined (refer to GB / T 3921-2008 and GB / T3921-2008), and the results are shown in Table 3; the antibacterial property of the fabric is tested (refer to GB / T 20944.3-2008), far-infrared heating performance (refer to GB / T 30127-2013), negative ion generation (refer to GB / T30128-2013), old age odor elimination function (refer to GB / T 33610.1-2019), antistatic performance (refer to GB / T12703.4-2010), and ultraviolet protection performance (refer to GB / T 18830-2009) as shown in Table 4; the data show that the graphene functional fabric has excellent properties and reliable processing and use fastness; the special two-dimensional structure of graphene makes it have mechanical, electrical, thermal, chemical and other properties that conventional macroscopic materials cannot match, and it has been well known to scientific and technological workers. After being compounded with pure cotton yarn, it gives it the above functionality; the high adsorption capacity and excellent composite fastness come from the processing technology designed by this method; the surface of graphene oxide has rich hydroxyl, carboxyl and epoxy oxygen-containing groups, which has good dispersibility in water, and the presence of polar groups makes it have a higher affinity with cotton yarn, so a higher adsorption capacity can be obtained; after being adsorbed on the yarn, the oxygen-containing groups on the surface of graphene disappear through the reduction step, and the hydrophobic nature is restored, embedded in the fiber, which makes it have better wet treatment fastness; in addition, the unique two-dimensional nanostructure of graphene also gives it high directness, and the small size effect and surface effect may obtain a stronger combination with the fiber.

[0095] Experimental Example 2:

[0096] The functional graphene yarn obtained in the above embodiment 1 is used to prepare the functional woven fabric, specifically: the functional graphene yarn is divided into yarns, the functional graphene yarn after the division is wound into cones, and the functional graphene yarn cones are weaved to obtain the functional woven fabric.

[0097] Experimental Example 3:

[0098] The functional nonwoven sheet is prepared using the functional graphene yarn obtained in the above Example 1, specifically: the graphene cotton yarn is combed into a uniform fiber web, and the fibers in the fiber web are softened and bonded together by a thermal consolidation method to obtain a functional nonwoven sheet.

[0099] Table 1 Colorimetric data of functional graphene yarn

[0100] project L* a* b* C* ho DE* data 43.78 0.92 2.66 2.81 71.02 48.15

[0101] Table 2 Comparison of mechanical properties of ordinary yarn and functional yarn

[0102] Breaking strength / N Elongation at break / % Ordinary yarn 329.53 6.27 Functional Yarn 309.55 5.92

[0103] Table 3 Composite fastness of graphene and yarn (knitted fabric)

[0104]

[0105] Table 4 Functional characterization of graphene functional pure cotton fabrics

[0106]

[0107]

[0108] Based on the above, the advantage of the present invention is that when the invention is used, graphene oxide is compounded with yarn in a stacking manner, and functional graphene yarn is obtained after reduction. The yarn not only retains the original softness, breathability and moisture absorption properties of cotton fiber, but also has excellent conductivity, antibacterial property, anti-ultraviolet function, far-infrared emission function, and negative ion generation function.

[0109] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A method for applying graphene to natural cotton textile materials, comprising the following steps: Step 1, preparing graphene oxide solution; Step 2, impregnating cotton yarn; Step 3, adding additives; Step 4, stacking yarn; Step 5, heating yarn; Step 6, reduction treatment; Step 7, soaping treatment; Step 8, washing and drying; It is characterized in that: Step 1: preparing a graphene oxide solution with a concentration of 1-10% and a bath ratio of 1:5-50, and performing ultrasonic dispersion treatment on the graphene oxide solution; Step 2: immersing the yarn in the graphene oxide solution after ultrasonic dispersion treatment in step 1; Step three is: adding an inorganic salt and a dispersant to the graphene oxide solution in step two, and continuing to immerse the yarn in the graphene oxide solution; Step 4 is: taking out the yarn impregnated in step 3, stacking for 4-48 hours, repeating the impregnation and stacking steps 1-3 times, so that the amount of liquid in the yarn is controlled at 80-150%; Step 5: taking out the yarn piled in step 4 and heating it at 65-160° C. for 3-50 minutes; Step six is: taking out the yarn after the heating treatment in step five and immersing it in the reducing solution; Step seven is: taking out the yarn after the reduction treatment in step six and performing soap washing; Step eight is: taking out the yarn after the soaping treatment in step seven, washing and drying the yarn to obtain functional graphene yarn.

2. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step 1, the lateral size of the graphene oxide is 100 nm-50 μm, and the number of layers is 1-9.

3. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step 1, the ultrasonic dispersion treatment time is 10-240 min.

4. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step 2, the yarn includes pure cotton yarn and blended yarn containing natural cotton, and the yarn is impregnated for 1-30 minutes.

5. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step three, the inorganic salt is one or more of nitrate, sulfate, phosphate, and chloride, and the concentration is 1-100 times the concentration of graphene. The dispersant is one or more of anionic dispersants and non-ionic dispersants, and the concentration is 0.01-10 g / L. The immersion time of the yarn is 1-30 min.

6. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step six, the immersion temperature is 50-100° C., and the immersion time is 3-100 min.

7. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step six, the reducing solution is prepared by using 1-15 g / L of alkali agent and 1-15 g / L of reducing powder, and the bath ratio is 1:5-50.

8. The method for applying graphene to natural cotton textile materials according to claim 7, characterized in that: The alkali agent is one or more of hydroxide, phosphate, carbonate, sulfate and ammonia soluble alkali.

9. The method for applying graphene to natural cotton textile materials according to claim 7, characterized in that: The reducing powder is one or more of metal complexing agents, divalent sulfur compounds, sulfites, vitamins, and hydrazine compounds.

10. The method for applying graphene to natural cotton textile materials according to claim 1, characterized in that: In the step 7, the bath ratio used in the soaping treatment is 1:5-50, the soap flake concentration is 1-20 g / L, the soaping temperature is 50-100° C., and the soaping time is 5-240 min.

Citation Information

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