A flexible heating safety protective webbing and its manufacturing process

Abstract

This application relates to the field of safety protective webbing technology, specifically disclosing a flexible heating safety protective webbing and its manufacturing process. The flexible heating safety protective webbing is mainly made of polyester fiber yarn and graphene fiber through blending, weaving, and setting. The graphene fiber yarn is mainly made from the following raw materials: polyethylene terephthalate, modified graphene microsheets, ammonium polyphosphate, compatibilizer, and antioxidant. The modified graphene microsheets are prepared by grafting graphene microsheets with 1,3-divinyltetraethoxydisilazane, trimethylolpropane triacrylate, and triethylenetetramine. This graphene fiber yarn has the advantages of high breaking strength and uniform appearance, and the resulting flexible heating safety protective webbing has the advantages of high wear resistance and high antibacterial properties, while also having a smooth appearance, soft touch, and durability, meeting market demands.

Description

Technical Field

[0001] This application relates to the field of safety protection webbing technology, and more specifically, it relates to a flexible heating safety protection webbing and its manufacturing process. Background Technology

[0002] Webbing is a narrow-width or tubular fabric made from various yarns, widely used in clothing, footwear, bags, industry, agriculture, transportation, and other fields. Flexible safety webbing is a type of webbing primarily used for protection, such as fire safety webbing, high-altitude work safety webbing, and automotive safety webbing. Most flexible safety webbing on the market is made from polyester, nylon, polypropylene, spandex, and other fiber yarns, woven together. Some researchers, in order to enable flexible safety webbing to generate heat, have proposed modifying the fiber yarn with graphene dispersion and grafting graphene onto the fiber yarn surface to obtain graphene fiber yarn. They believe that the thermal conductivity of graphene would allow the flexible safety webbing to generate heat. However, in actual research, the applicant found that while immersing the fiber yarn in graphene dispersion can achieve the grafting purpose, it requires a long soaking time for the graphene to stabilize and graft. This prolonged soaking time reduces the tensile strength of the fiber yarn, affecting the weaving of the graphene fiber yarn and ultimately impacting the usability of the flexible heating safety webbing. Summary of the Invention

[0003] This application provides a flexible heating safety protective webbing and its manufacturing process. Graphene micro-flakes are added to the raw material of graphene fiber yarn, and the graphene micro-flakes are modified. This not only increases the stability of the graphene micro-flakes in the graphene fiber yarn, but also provides a heating effect. At the same time, it also makes the graphene fiber yarn exhibit the advantages of high breaking strength and uniform appearance.

[0004] In the first aspect, this application provides a flexible heat-generating safety protective webbing, which adopts the following technical solution:

[0005] A flexible heating safety protective webbing, which is mainly made of polyester fiber yarn and graphene fiber through blending, weaving and shaping;

[0006] The graphene fiber yarn is mainly made of the following raw materials in parts by weight: 65-75 parts of polyethylene terephthalate, 25-35 parts of modified graphene microsheets, 1-3 parts of ammonium polyphosphate, 2-4 parts of compatibilizer, and 1-3 parts of antioxidant; the modified graphene microsheets are prepared by grafting graphene microsheets with 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine.

[0007] The graphene fiber yarn of this application incorporates ammonium polyphosphate in polyethylene terephthalate (PET), which provides flame retardancy and enhances the safety of the graphene fiber yarn. Adding graphene microflakes to PET not only increases the stability of the graphene microflakes within the graphene fiber yarn but also provides a heating effect. Furthermore, the graphene microflakes are modified to achieve a tensile strength >5 cN / dtex and yarn evenness <10%, exhibiting advantages such as high tensile strength and uniform appearance. Simultaneously, the resulting flexible heating safety webbing exhibits abrasion resistance >40,000 cycles and a Staphylococcus aureus and Escherichia coli inhibition rate >99%, demonstrating high strength, high abrasion resistance, and high antibacterial properties, meeting market demands.

[0008] The modified graphene microsheets were prepared by grafting 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine. 1,3-divinyltetraethoxydisilane contains six siloxy groups and two carbon-carbon double bonds, allowing it to be directly grafted onto the surface and pores of the graphene microsheets. Trimethylolpropane triacrylate contains three carbon-carbon double bonds and three ester groups, enabling it to undergo polymerization with 1,3-divinyltetraethoxydisilane and be grafted onto the surface and pores of the graphene microsheets. Triethylenetetramine contains two amino groups and two secondary amino groups; the amino groups can undergo an amide reaction with the ester groups in trimethylolpropane triacrylate. By grafting 1,3-divinyltetraethoxydisilazane, trimethylolpropane triacrylate, and triethylenetetramine, a large number of active groups such as siloxy, amide, and amino groups are introduced onto the surface of graphene microflakes, significantly increasing the number of branches on the graphene microflakes. This enhances the bonding strength between the modified graphene microflakes and the raw material, improves the breaking strength of the graphene fiber yarn, reduces the evenness of the graphene fiber yarn, and thus increases the strength of the flexible heating safety webbing. Simultaneously, the modified graphene microflakes also possess excellent abrasion resistance and antibacterial properties, further enhancing the abrasion resistance and antibacterial properties of the flexible heating safety webbing.

[0009] Furthermore, the modified graphene microsheets are prepared using the following method:

[0010] T1. At a temperature of 60-70℃, graphene microsheets are added to N,N-dimethylformamide and ultrasonically treated for 20-40 min. Then, 1,3-divinyltetraethoxydisilane is added and stirred for 40-60 min. After that, trimethylolpropane triacrylate is added and stirred for 10-30 min. Then, an organic initiator is added and stirred for 1-3 h. After filtration and washing, a semi-finished product is obtained.

[0011] T2. At a temperature of 60-70℃, add the semi-finished product to N,N-dimethylformamide and stir for 10-30 minutes. Then add triethylenetetramine and stir for 7-9 hours. Filter, wash, and dry to obtain modified graphene microsheets.

[0012] Furthermore, the weight ratio of the graphene microsheets, 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, organic initiator, and triethylenetetramine is (10-20):(2-4):(2-4):(0.1-0.3):(1-3).

[0013] In the method for preparing modified graphene microsheets in this application, graphene microsheets are first dispersed in N,N-dimethylformamide, and then 1,3-divinyltetraethoxydisilane is added and grafted onto the surface and pores of the graphene microsheets. Next, trimethylolpropane triacrylate is added, which undergoes a polymerization reaction with 1,3-divinyltetraethoxydisilane under the action of an organic initiator, achieving grafting. The mixture is then filtered and washed to remove the organic initiator. The semi-finished product is then dispersed in N,N-dimethylformamide, and then triethylenetetramine, containing two amino groups, is added. These amino groups can undergo an amide reaction with the ester groups in trimethylolpropane triacrylate, also achieving grafting. By grafting 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine, the number of active groups and branches in graphene microsheets is greatly increased, enhancing the bonding strength between the modified graphene microsheets and the raw materials, improving the performance of the modified graphene microsheets, and increasing the breaking strength of graphene fiber yarn.

[0014] Furthermore, the organic initiator is one or more of dodecyl peroxide, benzoyl peroxide, and azobisisobutyronitrile. Preferably, the organic initiator is dodecyl peroxide.

[0015] Furthermore, the graphene microsheets undergo the following pretreatment before use:

[0016] Under inert gas protection, the graphene microsheets are heated to 1100-1200℃, and then carbon dioxide is introduced at a flow rate of 1000-2000mL / min. The temperature is maintained for 2-4 hours. After stopping the introduction of carbon dioxide, the temperature is cooled to room temperature under inert gas protection to obtain the pretreated graphene microsheets.

[0017] High-temperature calcination of graphene microsheets before use can effectively increase the porosity and active groups on the surface of the graphene microsheets, which facilitates the grafting modification of graphene microsheets, improves the modification effect and the use effect of modified graphene microsheets.

[0018] Preferably, the graphene microsheets undergo the following pretreatment before use:

[0019] Graphene microsheets were placed in an activation chamber, and nitrogen gas was continuously introduced to create a nitrogen-protected atmosphere within the chamber. The graphene microsheets were then heated to 1100℃. Nitrogen gas introduction was then stopped, and carbon dioxide was introduced at a flow rate of 1500 mL / min for 3 hours. Afterward, carbon dioxide introduction was stopped, but nitrogen gas was continuously introduced, and the chamber was cooled to room temperature to obtain pretreated graphene microsheets.

[0020] Furthermore, the graphene microsheets have an average particle size of 10-30 μm and a thickness of 8-25 nm. Preferably, the graphene microsheets have an average particle size of 10-20 μm and a thickness of 8-15 nm. More preferably, the graphene microsheets have an average particle size of 15 μm and a thickness of 13 nm.

[0021] Furthermore, the polyethylene terephthalate is one or more of PET RE5264, PET RE5329, and PET RE5333. Preferably, the polyethylene terephthalate is PET RE5329.

[0022] Furthermore, the compatibilizer is an ethylene-acrylate-glycidyl methacrylate terpolymer. Preferably, the ethylene-acrylate-glycidyl methacrylate terpolymer is ethylene-acrylate-glycidyl methacrylate terpolymer AX8900.

[0023] Furthermore, the antioxidant is one or more of antioxidant 264, antioxidant 168, and antioxidant 1010. Preferably, the antioxidant is either antioxidant 264 or antioxidant 168, and the weight ratio of antioxidant 264 to antioxidant 168 is (1-3):(1-3). More preferably, the weight ratio of antioxidant 264 to antioxidant 168 is 1:1.

[0024] Furthermore, the graphene fiber yarn is prepared by the following method: polyethylene terephthalate, modified graphene microsheets, ammonium polyphosphate, compatibilizer, and antioxidant are mixed, melted, spun, cured, stretched, and dried to obtain graphene fiber yarn.

[0025] Graphene fiber yarn is obtained by directly mixing the raw materials, then melting, spinning, curing, stretching, and drying. This method makes the preparation of graphene fiber yarn simple and stable.

[0026] Secondly, this application provides a manufacturing process for the aforementioned flexible heat-generating safety protective webbing, employing the following technical solution:

[0027] A manufacturing process for the aforementioned flexible heat-generating safety protective webbing includes the following steps:

[0028] S1. Weaving: Polyester fiber yarn and graphene fiber yarn are blended and woven to obtain a webbing preform.

[0029] S2. Heat setting: Heat the webbing blank to 40-60℃ and keep it at that temperature for 1-3 minutes. Then heat it to 120-180℃ and keep it at that temperature for 2-5 minutes. After that, spray it with water and dehydrate it under vacuum to obtain the set webbing.

[0030] S3. Post-processing: Immerse the shaped webbing in a polymethylsiloxane solution, remove and dry to obtain a flexible heat-generating safety protective webbing.

[0031] The production process of this application involves first weaving, then heat setting, followed by immersion in a polymethylsiloxane solution for surface treatment. Through the coordination of these steps, the flexible heating safety webbing is not only easier to process, but the high-temperature setting also increases stability. Simultaneously, the surface treatment with the polymethylsiloxane solution forms a coating on the surface of the set webbing, increasing the service life of the flexible heating safety webbing.

[0032] Furthermore, the weight ratio of the polyester fiber yarn to the graphene fiber yarn is (80-90):(10-20). Preferably, the weight ratio of the polyester fiber yarn to the graphene fiber yarn is 85:15.

[0033] Furthermore, the fineness of polyester fiber yarn is 100-200D; the fineness of graphene fiber yarn is 100-200D.

[0034] Furthermore, the polymethylsiloxane solution is mainly composed of the following raw materials in weight percentages: 90-93% polymethylsiloxane emulsion and 3-10% water. Preferably, the polymethylsiloxane emulsion is a polydimethylsiloxane emulsion. More preferably, the polymethylsiloxane emulsion is polymethylsiloxane emulsion SM2011.

[0035] In summary, this application has at least the following beneficial effects:

[0036] 1. The flexible heating safety protective webbing of this application is mainly made of polyester fiber yarn and graphene fiber through blending, weaving and shaping. Through the mutual cooperation of polyester fiber yarn and graphene fiber yarn, the flexible heating safety protective webbing has a wear resistance of >40,000 times, a Staphylococcus aureus inhibition rate of >99%, and an Escherichia coli inhibition rate of >99%, showing the advantages of high strength, high wear resistance and high antibacterial properties. Moreover, it has a smooth appearance, soft touch, and durability, meeting market demand.

[0037] 2. Adding graphene microflakes to the raw materials of graphene fiber yarn not only increases the stability of the graphene microflakes in the graphene fiber yarn, but also provides a heating effect. Furthermore, combined with the modification treatment of the graphene microflakes, a large number of active groups such as siloxy groups, amide groups, and amino groups are introduced onto the surface of the graphene microflakes, and the number of branches on the graphene microflakes is greatly increased. This results in graphene fiber yarn with a breaking strength >5cN / dtex and evenness <10%, exhibiting advantages such as high breaking strength and uniform appearance. Implementation

[0038] To make this application easier to understand, the following detailed description will be provided with reference to embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of application of this application. Unless otherwise specified, the raw materials or components used in this application can be obtained commercially or by conventional methods.

[0039] Preparation Example

[0040] Preparation Example 1

[0041] A modified graphene microsheet is prepared by the following method:

[0042] T0. Place 15 kg of graphene microsheets in an activation chamber, then continuously purge with nitrogen gas to create a nitrogen-protected atmosphere in the chamber. Next, heat the graphene microsheets to 1100℃. Then, stop the nitrogen purge and purge with carbon dioxide at a flow rate of 1500 mL / min, maintaining the temperature for 3 hours. Afterward, stop the carbon dioxide purge and continue purging with nitrogen gas, cooling to 25℃ to obtain the pretreated graphene microsheets.

[0043] The graphene microflakes have an average particle size of 15μm and a thickness of 13nm, and are selected from Guangzhou Hongwu Materials Technology Co., Ltd.

[0044] T1. At a temperature of 65℃, pretreated graphene microsheets obtained in step T0 were added to 100 kg of N,N-dimethylformamide and sonicated for 30 min. Then, 3 kg of 1,3-divinyltetraethoxydisilane was added and stirred for 50 min. Next, 3 kg of trimethylolpropane triacrylate was added and stirred for 20 min. Then, 0.2 kg of dodecyl peroxide was added and stirred for 2 h. The mixture was then filtered, washed, and dried to obtain a semi-finished product.

[0045] T2. At a temperature of 65℃, the semi-finished product obtained in step T1 was added to 100 kg of N,N-dimethylformamide and stirred for 20 min. Then, 2 kg of triethylenetetramine was added and stirred for 8 h. After filtration, washing, and drying, modified graphene microsheets were obtained.

[0046] Preparation Example 2

[0047] A modified graphene microsheet differs from Preparation Example 1 in that the amounts of graphene microsheet, 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, dodecyl peroxide, and triethylenetetramine added are different.

[0048] Furthermore, the amount of graphene micro flakes added is 10 kg, the amount of 1,3-divinyltetraethoxydisilane added is 2 kg, the amount of trimethylolpropane triacrylate added is 4 kg, the amount of dodecyl peroxide added is 0.1 kg, and the amount of triethylenetetramine added is 3 kg.

[0049] Preparation Example 3

[0050] A modified graphene microsheet differs from Preparation Example 1 in that the amounts of graphene microsheet, 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, dodecyl peroxide, and triethylenetetramine added are different.

[0051] Furthermore, the amount of graphene micro flakes added is 20 kg, the amount of 1,3-divinyltetraethoxydisilane added is 4 kg, the amount of trimethylolpropane triacrylate added is 2 kg, the amount of dodecyl peroxide added is 0.3 kg, and the amount of triethylenetetramine added is 1 kg. Example

[0052] Table 1. Content of each raw material in graphene fiber yarn (unit: kg)

[0053] Example Example 1 Example 2 Example 3 polyethylene terephthalate 70 65 75 Modified graphene microplates 30 35 25 Ammonium polyphosphate 2 3 1 compatibilizer 3 2 4 antioxidants 2 1 3 Example

[0054] A graphene fiber yarn, the raw materials and their proportions are shown in Table 1.

[0055] Among them, polyethylene terephthalate is PET RE5329, selected from Ningbo Rongsu New Material Co., Ltd.; ammonium polyphosphate is ammonium polyphosphate JD-657, selected from Dongying Jingdong Chemical Co., Ltd.; compatibilizer is ethylene-acrylate-glycidyl methacrylate terpolymer, selected from Arkema AX8900; antioxidants are antioxidant 264 and antioxidant 168, and the weight ratio of antioxidant 264 and antioxidant 168 is 1:1; the modified graphene microsheets are prepared by the method of Preparation Example 1.

[0056] A method for preparing graphene fiber yarn includes the following steps:

[0057] Modified graphene microsheets, ammonium polyphosphate, compatibilizer, and antioxidant were added to polyethylene terephthalate and stirred for 30 minutes. Then, the mixture was melted, spun, cured, stretched, and dried to obtain graphene fiber yarn.

[0058] The melting temperature is 220℃, and the fineness of the graphene fiber yarn is 150D. Example

[0059] A graphene fiber yarn differs from Example 1 in that the raw material ratio of the graphene fiber yarn is different, as shown in Table 1. Example

[0060] A graphene fiber yarn differs from Example 1 in that the raw material ratio of the graphene fiber yarn is different, as shown in Table 1. Example

[0061] A graphene fiber yarn differs from Example 1 in that the source of the modified graphene microsheets in the raw materials of the graphene fiber yarn is different; the modified graphene microsheets are prepared using the method of Preparation Example 2. Example

[0062] A graphene fiber yarn differs from Example 1 in that the source of the modified graphene microsheets in the raw materials of the graphene fiber yarn is different; the modified graphene microsheets are prepared using the method of Preparation Example 3.

[0063] Comparative Example

[0064] Comparative Example 1

[0065] A graphene fiber yarn, which differs from Example 1 in that the modified graphene microsheets are replaced with an equal amount of graphene microsheets in the raw materials of the graphene fiber yarn.

[0066] Comparative Example 2

[0067] A graphene fiber yarn differs from that of Example 1 in that, in the raw material of the graphene fiber yarn, an equal amount of pretreated graphene microsheets replaces the modified graphene microsheets. The pretreated graphene microsheets are prepared using the method in step T0 of Preparation Example 1.

[0068] Comparative Example 3

[0069] A graphene fiber yarn, which differs from Example 1 in that, in the preparation method of modified graphene microsheets, an equal amount of 1,3-divinyltetraethoxydisilane replaces trimethylolpropane triacrylate and triethylenetetramine.

[0070] Comparative Example 4

[0071] A graphene fiber yarn differs from Example 1 in that, in the modified graphene microsheet preparation method, an equal amount of trimethylolpropane triacrylate is used to replace 1,3-divinyltetraethoxydisilane and triethylenetetramine.

[0072] Comparative Example 5

[0073] A graphene fiber yarn differs from Example 1 in that, in the modified graphene microsheet preparation method, an equal amount of triethylenetetramine replaces 1,3-divinyltetraethoxydisilane and trimethylolpropane triacrylate in the raw materials of the graphene fiber yarn.

[0074] Application examples

[0075] Application Example 1

[0076] A flexible heating safety protective webbing is made of polyester fiber yarn and graphene fiber through blending, weaving and shaping.

[0077] A manufacturing process for a flexible heat-generating safety protective webbing includes the following steps:

[0078] S1. Weaving: Polyester fiber yarn and graphene fiber yarn are blended and woven to obtain a ribbon preform.

[0079] The weight ratio of polyester fiber yarn to graphene fiber yarn is 85:15, and the fineness of the polyester fiber yarn is 150D; the fineness of the graphene fiber yarn is 150D, and the graphene fiber yarn is prepared by the method of Example 1.

[0080] S2. Heat setting: The webbing blank obtained in step S1 is heated to 50°C and held for 2 minutes. Then, the temperature is increased to 120°C and held for 3.5 minutes. After that, it is washed with water spray and vacuum dehydrated to obtain the set webbing.

[0081] S3. Post-processing: The shaped webbing obtained in step S2 is immersed in a polymethylsiloxane solution at 35°C for one dip and one roll, with a liquor ratio of 1:10 and a roll-off rate of 85%. Then it is dried at 120°C to obtain a flexible heat-generating safety protective webbing.

[0082] The polymethylsiloxane solution is mainly composed of polymethylsiloxane emulsion and water, with the weight addition of polymethylsiloxane emulsion being 4% and water being 96%. The polymethylsiloxane emulsion is a polydimethylsiloxane emulsion, specifically SM2011 from Yantai Shunming New Materials Co., Ltd.

[0083] Application Example 2-5

[0084] A flexible heating safety protective webbing differs from Application Example 1 in that the source of the graphene fiber yarn is different, and the graphene fiber yarns of Application Examples 2-5 were prepared in accordance with Examples 2-5 respectively.

[0085] Comparative application examples

[0086] Compare and contrast examples 1-5

[0087] A flexible heating safety protective webbing differs from Application Example 1 in that the graphene fiber yarn has a different source, and the graphene fiber yarns of Comparative Application Examples 1-5 were prepared sequentially using Comparative Examples 1-5 respectively.

[0088] Performance testing

[0089] (1) The graphene fiber yarns obtained in Examples 1-5 and Comparative Examples 1-5 were taken as samples, and the following performance tests were performed on the samples. The test results are shown in Table 2.

[0090] The tensile strength of the specimens was tested in accordance with GB / T14344-2022 "Test Method for Tensile Properties of Chemical Fiber Filaments".

[0091] According to GB / T3292.2-2009 "Textiles - Test Methods for Yarn Unevenness - Part 2: Photoelectric Method", the unevenness of the yarn in the sample was tested.

[0092] (2) The flexible heating safety protective webbing obtained in Application Examples 1-5 and Comparative Application Examples 1-5 were taken as samples, and the following performance tests were performed on the samples. The test results are shown in Table 2.

[0093] In accordance with GB / T21196.2 "Textiles - Martindale Method - Determination of Abrasion Resistance of Fabrics - Part 2: Determination of Specimen Breakage", the number of rubbing cycles required for the specimen to breakage was tested.

[0094] According to GB / T20944.3-2008 "Evaluation of antimicrobial properties of textiles - Part 3: Shaking method", the inhibition rates of Staphylococcus aureus and Escherichia coli in the samples were tested.

[0095] Table 2 Test Results

[0096] Testing items Fracture strength / (cN / dtex) Unevenness of strips / (%) Testing items Wear resistance cycles (times) Staphylococcus aureus inhibition rate (%) Escherichia coli inhibition rate (%) Example 1 5.44 9.13 Application Example 1 ＞40000 99.5 99.6 Example 2 5.29 9.34 Application Example 2 ＞40000 99.4 99.5 Example 3 5.23 9.58 Application Example 3 ＞40000 99.3 99.6 Example 4 5.35 9.21 Application Example 4 ＞40000 99.4 99.4 Example 5 5.27 9.45 Application Example 5 ＞40000 99.3 99.5 Comparative Example 1 4.13 18.82 Comparative Application Example 1 ＞40000 99.3 99.4 Comparative Example 2 4.46 16.71 Comparative Application Example 2 ＞40000 99.5 99.6 Comparative Example 3 4.99 13.33 Comparative Application Example 3 ＞40000 99.4 99.5 Comparative Example 4 4.79 14.54 Comparative Application Example 4 ＞40000 99.3 99.5 Comparative Example 5 4.55 16.18 Comparative Application Example 5 ＞40000 99.4 99.4

[0097] As shown in Table 2, the graphene fiber yarn obtained in this application has high tensile strength, ranging from 5.23 to 5.44 cN / dtex, and also exhibits low yarn unevenness, ranging from 9.13% to 9.58%. This gives the graphene fiber yarn the advantages of high tensile strength and uniform appearance. The flexible heating safety webbing obtained in this application has high abrasion resistance, Staphylococcus aureus inhibition rate, and Escherichia coli inhibition rate. It has an abrasion resistance of >40,000 cycles, a Staphylococcus aureus inhibition rate of 99.3% to 99.5%, and an Escherichia coli inhibition rate of 99.4% to 99.6%. This gives the flexible heating safety webbing the advantages of high strength, high abrasion resistance, and high antibacterial properties.

[0098] Comparative Examples 1-3 were compared. In Comparative Example 1, graphene microflakes were added to the graphene fiber raw material; in Comparative Example 2, pretreated graphene microflakes were added to the graphene fiber raw material; and in Comparative Example 3, modified graphene microflakes were added to the graphene fiber raw material, and the graphene microflakes were grafted with 1,3-divinyltetraethoxydisilane. This shows that pretreatment of graphene microflakes, followed by further graft modification, can improve the breaking strength of graphene fiber yarn and reduce its unevenness.

[0099] Example 1 and Comparative Examples 3-5 were compared. In Comparative Example 3, the graphene microsheets were grafted with 1,3-divinyltetraethoxydisilane; in Comparative Example 4, the graphene microsheets were grafted with trimethylolpropane triacrylate; in Comparative Example 5, the graphene microsheets were grafted with triethylenetetramine; and in Example 1, the graphene microsheets were grafted with 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine. This demonstrates that the synergistic effect of 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine introduces a large number of active groups such as siloxy groups, amide groups, and amino groups onto the graphene surface, greatly increasing the number of branches in the graphene microsheets, enhancing the performance of the modified graphene microsheets, and enabling the graphene fibers to exhibit superior properties.

[0100] It should be noted that the embodiments described above are only for explaining this application and do not constitute any limitation on this application. This application has been described with reference to typical embodiments, but it should be understood that the terms used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to this application within the scope of the claims, and revisions can be made to the invention without departing from the scope and spirit of this application. Although the application described herein relates to specific methods, materials, and embodiments, it does not mean that this application is limited to the specific examples disclosed herein; on the contrary, this application can be extended to all other methods and applications with the same function.

Claims

1. A flexible heating safety protective webbing, characterized in that: It is mainly made of polyester fiber yarn and graphene fiber yarn through blending, weaving and setting; The graphene fiber yarn is mainly made of the following raw materials in parts by weight: 65-75 parts polyethylene terephthalate, 25-35 parts modified graphene microsheets, 1-3 parts ammonium polyphosphate, 2-4 parts compatibilizer, and 1-3 parts antioxidant; the modified graphene microsheets are prepared by grafting graphene microsheets with 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, and triethylenetetramine. The modified graphene microsheets were prepared using the following method: S1: Place graphene microsheets in the activation chamber, then continuously purge with nitrogen gas to create a nitrogen-protected environment in the activation chamber; then heat the graphene microsheets to 1100℃; then stop purging with nitrogen gas and purge with carbon dioxide at a flow rate of 1500mL / min, and maintain the temperature for 3 hours; then stop purging with carbon dioxide gas and continuously purge with nitrogen gas, and cool down to room temperature to obtain pretreated graphene microsheets. S2. At a temperature of 60-70℃, pretreated graphene microsheets are added to N,N-dimethylformamide and ultrasonically treated for 20-40 min. Then, 1,3-divinyltetraethoxydisilane is added and stirred for 40-60 min. After that, trimethylolpropane triacrylate is added and stirred for 10-30 min. Then, an organic initiator is added and stirred for 1-3 h. The mixture is filtered, washed, and a semi-finished product is obtained. S3. At a temperature of 60-70℃, add the semi-finished product to N,N-dimethylformamide and stir for 10-30 minutes. Then add triethylenetetramine and stir for 7-9 hours. Filter, wash, and dry to obtain modified graphene microsheets. The weight ratio of the graphene microsheets, 1,3-divinyltetraethoxydisilane, trimethylolpropane triacrylate, organic initiator, and triethylenetetramine is (10-20):(2-4):(2-4):(0.1-0.3):(1-3).

2. The flexible heating safety webbing according to claim 1, characterized in that: The graphene microflakes have an average particle size of 10-30 μm and a thickness of 8-25 nm.

3. A flexible heating safety webbing according to claim 1, characterized in that: The polyethylene terephthalate is one or more of PET RE5264, PET RE5329, and PET RE5333; The compatibilizer is an ethylene-acrylate-glycidyl methacrylate terpolymer; The antioxidant is one or more of antioxidants 264, 168, and 1010.

4. The flexible heating safety protective webbing according to claim 1, characterized in that: The graphene fiber yarn is prepared by the following method: polyethylene terephthalate, modified graphene microsheets, ammonium polyphosphate, compatibilizer, and antioxidant are mixed, melted, spun, cured, stretched, and dried to obtain graphene fiber yarn.

5. A manufacturing process for a flexible heat-generating safety protective webbing as described in any one of claims 1-4, characterized in that: Includes the following steps: S1. Weaving: Polyester fiber yarn and graphene fiber yarn are blended and woven to obtain a webbing preform. S2. Heat setting: Heat the webbing blank to 40-60℃ and keep it at that temperature for 1-3 minutes. Then heat it to 120-180℃ and keep it at that temperature for 2-5 minutes. After that, spray it with water and dehydrate it under vacuum to obtain the set webbing. S3. Post-processing: Immerse the shaped webbing in a polymethylsiloxane solution, remove and dry to obtain a flexible heat-generating safety protective webbing.

6. The manufacturing process of a flexible heating safety protective webbing according to claim 5, characterized in that: The weight ratio of the polyester fiber yarn to the graphene fiber yarn is (80-90):(10-20).

7. The manufacturing process of a flexible heating safety protective webbing according to claim 5, characterized in that: The polymethylsiloxane solution is mainly made from the following raw materials in weight percentages: 90-93% polymethylsiloxane emulsion and 3-10% water.