Composite Lyocell / Bamboo Fiber Healthcare Fabric with Flame Retardant and Negative Ion Generating Properties

Abstract

The objective of the present invention is to provide a method for manufacturing a composite lyocell / bamboo fiber health care fabric that has flame retardancy and negative ion generating properties. [Solution] The fabric manufacturing method involves first pretreating and pre-oxidizing lyocell fiber, then graft-copolymerizing acrylamide onto the surface of the lyocell fiber using a cerium salt initiator, chemically modifying the grafted modified fiber and phosphorylating it with diphenylphosphinous chloride to introduce a phosphorus-containing flame retardant onto the fiber surface, preparing flame-retardant lyocell fiber, and finally blending the flame-retardant lyocell fiber as the warp and the negative ion bamboo fiber as the weft through the following steps: fiber pretreatment → blending → cotton opening and dust removal → carding → drawing → roving → spinning → winding → warping → sizing → warp threading → weaving. The fabric of the present invention is environmentally friendly, flame-retardant, and has the effects of negative ion health care.

Description

[Technical Field]

[0001] The present invention relates to the field of flame-retardant fiber fabrics, and more particularly to a composite lyocell / bamboo fiber health care fabric with flame-retardant and negative ion generating properties and a manufacturing method thereof. [Background technology]

[0002] In recent years, with growing environmental awareness, regenerated cellulose fibers have gradually replaced various synthetic fibers, occupying an increasingly large proportion of our daily lives. Their applications have expanded from apparel and furniture to many other fields, including medicine, construction, and aerospace. Lyocell fiber is a new, environmentally friendly cellulose fiber. It uses N-methylmorpholine-N-oxide (NMMO) as a solvent, which has a very high recovery rate and can be recovered and reused after use, reducing environmental pollution and conserving resources. Its properties, including its smooth, comfortable hand feel and excellent breathability, make it a new, environmentally friendly fiber that is widely used in many industries, including apparel and interior design. However, like many textiles, lyocell is highly flammable, producing large amounts of smoke and high heat during combustion, posing a significant threat to human life and property. Therefore, improving the flame retardancy of regenerated cellulose fiber fabrics has attracted widespread attention, and research into the production of highly efficient and durable flame-retardant regenerated cellulose fibers has become a key challenge in the textile spinning industry. However, flame-retardant modification of textile fabrics currently faces the following main challenges: Flame retardants and additives used in flame-retardant fiber fabrics often lose their effectiveness over time and with increased washing, resulting in a decline in flame-retardant performance. Furthermore, many flame retardants can cause environmental pollution, especially halogen-based flame retardants, which can leave pollutants in the fabric and be released into the surrounding environment, resulting in significant environmental impact. Some flame retardants contain toxic substances, such as chlorine and bromine, which can potentially pose hazards to human health, including carcinogenicity and reproductive damage. Therefore, the development of a flame-retardant lyocell fabric that is simple, has stable flame retardancy, and is harmless to human health, is of great significance for the healthy development of mankind and the environment. Summary of the Invention [Problem to be solved by the invention]

[0003] The object of the present invention is to overcome the problems in the prior art by providing a composite lyocell / bamboo fiber healthcare fabric with flame retardant and negative ion generating properties, and a manufacturing method thereof. [Means for solving the problem]

[0004] In order to achieve the above object, the present invention employs the following technical means.

[0005] This composite lyocell / bamboo fiber health care fabric has flame retardancy and negative ion generating properties. The fabric is composed of lyocell fiber, bamboo fiber, and a phosphorus-containing flame retardant, the phosphorus-containing flame retardant being deposited on the surface of the lyocell fiber by surface graft copolymerization, and the bamboo fiber is a negative ion bamboo fiber, with the two fibers interwoven together. The fiber fabric has flame retardancy, and in vertical burning tests, it has an afterflame time of 0 seconds, a low burning rate of 1.6 mm / s, a char length of 48 mm, and a limiting oxygen index of 45.6%, and it also generates negative ions that are beneficial to human health.

[0006] The present invention focuses on fiber fabrics and develops a composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties, as well as a manufacturing method thereof. Ultimately, a composite lyocell / bamboo fiber health care fabric with strong flame retardancy and chemically stable flame retardancy and negative ion generating properties is obtained.

[0007] Compared with conventional flame-retardant modification methods (dipping and coating), graft copolymerization is an environmentally friendly and effective way to modify the chemical structure of textile surfaces. It allows polymer chains to be introduced onto the surface without destroying the overall structure of the textile. The strong covalent bonds between the grafted polymer chains and the fiber surface give the textile excellent durability. At the same time, by combining chemical modification with the introduction of phosphorus-containing flame retardants, the synergistic effect of phosphorus and nitrogen is achieved, improving the flame-retardant properties of the textile. Furthermore, by blending with negative ion bamboo fiber, we developed an environmentally friendly functional fiber fabric with flame retardant and negative ion-generating properties.

[0008] Preferably, the composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties is characterized in that the lyocell fiber is first immersed in a 5 wt% H2SO4 aqueous solution at 45°C for 30 minutes, then rinsed with distilled water until the rinse water becomes neutral, and then dried to a constant weight.

[0009] The lyocell fiber has a breaking strength of 3.9 cN / dtex, a CV value of breaking strength of 17.38%, a breaking elongation of 23.28%, a moisture regain of 4.58%, an average length of 37.0 mm, a volume resistivity of 8.3×10 5 Ω cm, and a linear density of 1.92 dtex.

[0010] The pH of the H2SO4 aqueous solution is 1, and the drying conditions are pre-drying in a thermostatic oven at 80°C for 5 minutes and baking at 160°C for 3 minutes.

[0011] Preferably, 30 ml of distilled water is added to a three-neck flask equipped with a constant pressure dropping funnel and a reflux condenser, the treated lyocell fiber is placed in the flask, the pH is adjusted to 2 with nitric acid, and the mixture is deoxygenated by purging with nitrogen gas for 30 minutes while stirring, and then cerium ammonium nitrate is added to pre-oxidize the fiber.

[0012] Preferably, an aqueous acrylamide solution is added dropwise, and the mixture is stirred at 45°C for 4 hours under a nitrogen gas atmosphere. After the reaction, fibers having a yellow viscous substance on the surface are obtained, which are then rinsed with distilled water and dried to a constant weight.

[0013] The concentration of the acrylamide aqueous solution is 40 wt %, and 10 ml of the solution is added dropwise.

[0014] Preferably, the treated lyocell fiber is placed in a three-neck flask containing tetrahydrofuran, and an appropriate amount of triethylamine is added as an acid binder. At the same time, a reflux condenser and a dropping funnel are attached, diphenylphosphinic acid chloride is placed in the dropping funnel, the tube is evacuated, and nitrogen gas is filled for protection. Then, diphenylphosphinic acid chloride is dropped and reacted in an ice bath for 6 hours. Then, the temperature is raised to 50°C, and the reaction is continued for 4 hours. After that, the fiber is taken out, rinsed repeatedly with water, and dried to a constant weight to obtain a flame-retardant modified lyocell fiber.

[0015] The ratio of triethylamine to diphenylphosphinous chloride used is 1:1.

[0016] Preferably, flame-retardant lyocell fiber is used as the warp yarn and negative ion bamboo fiber is used as the weft yarn, and the blended spinning process is fiber pretreatment → blending → cotton opening and dust removal → carding → drawing → roving → spinning → winding → warping → sizing → warp threading → weaving to obtain a composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties.

[0017] The negative ion bamboo fiber has a breaking strength of 2.29 cN / dtex, a CV value of breaking strength of 15.1%, a breaking elongation of 24.2%, a moisture content of 12.8%, an average length of 37.9 mm, a linear density of 1.31 dtex, and a negative ion concentration of 1060 cm -3 is.

[0018] The flame-retardant lyocell fiber and negative ion bamboo fiber are loosened in advance, then uniformly sprayed with an antistatic agent mixture and left to stand for 12 hours or more. The mass ratio of the antistatic agent to water in the antistatic agent mixture is 1:30.

[0019] In the weaving process, a 5-ply, 3-step twill weave is designed, with a warp density of 685 threads / 10cm, a weft density of 433 threads / 10cm, and a width of 330cm.

[0020] Preferably, the thermal stability of the composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generation properties is measured by thermogravimetric analysis (TG). A YG(13)815D-I (vertical method) fabric flame retardancy tester is used to test the vertical flame retardancy of the fabric in accordance with the requirements of GB / T 5455-1997 "Textile Flame Retardancy Test, Vertical Method." The ASTM D6413-08 (oxygen index method) fabric flame retardancy tester is used to test the flame retardancy of the fabric in accordance with the requirements of GB / T 5455-1997 "Textile Flame Retardancy Test, Oxygen Index Method," and the limiting oxygen index value is measured.

[0021] The sample mass in the TG measurement was 3 mg, the atmosphere was nitrogen gas, the temperature rise rate was 10°C / min, and the temperature rise range was 0 to 800°C.

[0022] To measure the limiting oxygen index, a test specimen is clamped vertically in a transparent combustion cylinder with oxygen and nitrogen gases flowing upward using a test specimen holder, the top of the test specimen is ignited, and the subsequent combustion phenomenon is observed. The duration and length of combustion are compared with the specified limit values, and the afterglow time is recorded. The limiting oxygen index value can be determined through a series of test results at different oxygen concentrations.

[0023] The flame-retardant, negative-ion-generating fiber fabric produced by this invention is a composite of flame-retardant lyocell fiber and negative-ion bamboo fiber. The flame-retardant lyocell fiber is prepared by graft copolymerization with an acrylamide intermediate, followed by phosphorus-containing flame retardants and phosphorylation. This results in a lyocell fiber with a synergistic flame-retardant effect of phosphorus and nitrogen. By interweaving this with negative-ion bamboo fiber, the flame-retardant properties of the fabric are improved, and its health-related functionality is enhanced. The vertical burn test results showed a flame after-time of 0 seconds, a low burning rate of 1.6 mm / s, and a char length of 48 mm. [Effects of the Invention]

[0024] Compared with the prior art, the technical means of the present invention produce the following advantageous technical effects:

[0025] 1. The present invention provides a composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties. The fabric is composed of flame-retardant modified lyocell fiber and negative ion bamboo fiber, which are acrylamide graft copolymerized / chemically modified. The acrylamide is deposited on the surface of the lyocell fiber by graft copolymerization, and a phosphorus-containing flame retardant is grafted to the acrylamide by chemical method, which enhances the flame retardancy of the fiber. The blending of negative ion bamboo fiber also improves the healthcare functionality of the fabric.

[0026] 2. Acrylamide graft copolymerization is a method of introducing acrylamide into cellulose fibers through the reaction between the hydroxyl groups on the cellulose polymer and the amino groups on the acrylamide, and then chemically modifying the fibers to incorporate phosphorus-containing flame retardants, thereby enhancing flame retardancy. This method provides long-lasting and stable flame retardancy.

[0027] 3. Vertical combustion tests demonstrated that the composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties provided by the present invention has excellent flame retardancy, with a limiting oxygen index of 45.6% and maintaining a limiting oxygen index of 39.1% even after 30 washes. This demonstrates that the composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties provided by the present invention has excellent flame retardancy. [Brief explanation of the drawings]

[0028] [Figure 1] 1 is a flowchart of the manufacturing process of a composite lyocell / bamboo fiber health care fabric with flame retardant and negative ion generating properties. DETAILED DESCRIPTION OF THE INVENTION

[0029] The following examples will explain in detail the composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties provided by the present invention and its manufacturing method. The following examples are used only to explain the present invention and should not be understood as limiting the scope of protection of the present invention. It should be noted that those skilled in the art can specifically implement the present invention by making non-essential improvements and adjustments based on the above-mentioned invention content and still fall within the scope of protection of the present invention.

[0030] Example 1 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, cerium ammonium nitrate, 40wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0031] Samples were prepared based on the above formulation, and the specific steps were as follows.

[0032] (1) First, the lyocell fiber was immersed in a 5 wt% H2SO4 aqueous solution at 45°C for 30 minutes, then rinsed with distilled water until the rinse solution became neutral, and then dried to a constant weight. 30 ml of distilled water was added to a three-neck flask equipped with a constant-pressure dropping funnel and a reflux condenser, and the treated lyocell fiber was placed in it. The pH was adjusted to 2 with nitric acid, and the mixture was deoxygenated by purging with nitrogen gas for 30 minutes while stirring. Then, cerium ammonium nitrate was added to pre-oxidize the fiber.

[0033] (2) A 40 wt% aqueous acrylamide solution was added dropwise, and the mixture was stirred at 45°C for 4 hours under a nitrogen gas atmosphere. After the reaction, fibers with a yellow viscous substance on the surface were obtained. The fibers were rinsed with distilled water and then dried to a constant weight.

[0034] (3) The above-mentioned treated lyocell fiber was placed in a three-neck flask containing tetrahydrofuran, and triethylamine was added as an acid binder. At the same time, a reflux condenser and a dropping funnel were attached, and diphenylphosphinic acid chloride was placed in the dropping funnel. The tube was evacuated and filled with nitrogen gas for protection. Then, diphenylphosphinic acid chloride was added dropwise, and the ratio of triethylamine to diphenylphosphinic acid chloride was 1:1. The mixture was reacted in an ice bath for 6 hours, and then the temperature was raised to 50°C and the mixture was reacted for 4 hours. After that, the fiber was taken out, rinsed repeatedly with water, and dried to a constant weight to obtain a flame-retardant modified lyocell fiber.

[0035] (4) Flame-retardant lyocell fiber is used as the warp thread and negative ion bamboo fiber is used as the weft thread, and the spinning process is as follows: fiber pretreatment → blending → opening and dust removal → carding → drawing → roving → fine spinning → winding → warping → sizing → warp threading → weaving.

[0036] Example 2 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, ceric ammonium nitrate, 0wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0037] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0038] Example 3 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, ceric ammonium nitrate, 10wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0039] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0040] Example 4 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, cerium ammonium nitrate, 20wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0041] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0042] Example 5 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, cerium ammonium nitrate, 30wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0043] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0044] Example 6 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, ceric ammonium nitrate, 50wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0045] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0046] Example 7 This embodiment provides a composite Lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties and a manufacturing method thereof, and the composition is as follows: Lyocell fiber, 5wt% H2SO4 aqueous solution, nitric acid, ceric ammonium nitrate, 60wt% acrylamide aqueous solution, tetrahydrofuran, triethylamine, diphenylphosphinic acid chloride, negative ion bamboo fiber.

[0047] Samples were prepared based on the above formulation, and the specific steps are shown in Example 1.

[0048] (Comparative Example 1) In this comparative example, a lyocell / bamboo fiber healthcare fabric was manufactured using non-flame retardant modified lyocell fiber. The specific process is as follows:

[0049] Lyocell fiber is used as the warp thread and negative ion bamboo fiber is used as the weft thread, and the spinning process is as follows: fiber pre-treatment → blending → opening and dust removal → carding → drawing → roving → spinning → winding → warping → sizing → warp threading → weaving.

[0050] The samples of Examples 1 to 7 were subjected to TG measurement.

[0051] [Table 1]

[0052] As the acrylamide content increased, the decomposition starting temperature, the decomposition temperature at which the weight loss rate reached its maximum, the decomposition end temperature, and the carbon residue rate all increased significantly, indicating that the thermal stability of the fabric improved. This indicates that the flame retardancy of lyocell fiber can be modified through cellulose-grafted polyacrylamide and diphenylphosphinous chloride, which can change the thermal decomposition process of lyocell fiber and effectively improve the flame retardancy of lyocell fiber.

[0053] The samples of Examples 1 to 7 were subjected to a vertical flammability test and limiting oxygen index measurement.

[0054] [Table 2]

[0055] Acrylamide acts as an intermediate to graft phosphorus-containing flame retardants onto the fiber surface. Therefore, as the acrylamide concentration increases, the content of phosphorus-containing flame retardants on the fiber surface increases, improving flame retardancy and limiting oxygen index. After the acrylamide content was increased to 40 wt% (Examples 1, 6, and 7), the flame retardancy and limiting oxygen index of the fiber fabric did not improve further. This is mainly because the acrylamide content at this level was sufficient to graft all of the added phosphorus-containing flame retardant onto the fiber surface, and further increases in the acrylamide content did not significantly improve the flame retardancy of the fabric.

[0056] The fabrics of Example 1 and Comparative Example 1 were subjected to a vertical combustion test and limiting oxygen index measurement.

[0057] [Table 3]

[0058] When ignited in air, the untreated fabric burned quickly, burning for 4 seconds with no char left behind. The treated fabric did not continue to burn after a 30-second ignition test and the ignition source was removed, leaving behind a large amount of char. This indicates that the introduction of flame retardants significantly improved the fire resistance of the fabric. Its limiting oxygen index was also significantly improved. Even after 30 washes, the limiting oxygen index remained at 39.1%, far higher than that of the untreated fabric.

[0059] These specific examples are merely for clarifying the technical content of the present invention and are not intended to limit the present invention. After reading this specification, a person skilled in the art may make non-creative modifications to these examples as necessary, but such modifications should be protected by patent law as long as they fall within the scope of the claims of the present invention.

Claims

1. A composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties, characterized in that it is made of flame retardant modified lyocell fiber and bamboo fiber, acrylamide is introduced to the surface of the lyocell fiber by graft copolymerization, and a phosphorus-containing flame retardant is further introduced by phosphorylation, the bamboo fiber is negative ion bamboo fiber, and the composite fabric is produced by interweaving the flame retardant lyocell fiber and the negative ion bamboo fiber.

2. First, lyocell fiber was mixed with 4 to 6 wt% H ２ SO ４ The composite lyocell / bamboo fiber healthcare fabric with flame retardancy and negative ion generating properties according to claim 1, characterized in that the fabric is immersed in an aqueous solution at 0 to 50°C for 25 to 35 minutes, then rinsed with distilled water until the rinse water becomes neutral, and dried to a constant weight.

3. The composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties according to claim 2, characterized in that 25-35 ml of distilled water is added to a three-necked flask equipped with a constant pressure dropping funnel and a reflux condenser, the treated lyocell fiber is added, the pH is adjusted to 1.5-2.5 with nitric acid, and the mixture is deoxygenated by purging with nitrogen gas for 25-35 minutes while stirring, and then cerium ammonium nitrate is added to pre-oxidize the fiber.

4. The composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties according to claim 3, characterized in that a 30-50 wt % acrylamide aqueous solution is added dropwise, and the mixture is stirred at 40-50°C for 3-5 hours under a nitrogen gas atmosphere, and after the reaction, a fiber with a yellow viscous substance on the surface is obtained, which is rinsed with distilled water and then dried to a constant weight.

5. The composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties according to claim 4, characterized in that the treated lyocell fiber is placed in a three-neck flask containing tetrahydrofuran, triethylamine is added as an acid binder, and at the same time, a reflux condenser and a dropping funnel are attached, diphenylphosphinic chloride is placed in the dropping funnel, the tube is evacuated, and nitrogen gas is filled to protect it, and then diphenylphosphinic chloride is dropped in, with triethylamine and diphenylphosphinic chloride being used in a ratio of 1:1, and the reaction is carried out in an ice bath for 5-7 hours, and then the temperature is raised to 45-55°C and the reaction is carried out for 3-5 hours, after which the fiber is taken out, rinsed repeatedly with water, and dried to a constant weight to obtain a flame-retardant modified lyocell fiber.

6. The composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties according to claim 5, characterized in that the composite lyocell / bamboo fiber health care fabric with flame retardancy and negative ion generating properties is obtained by blending flame retardant lyocell fiber as the warp and negative ion bamboo fiber as the weft, and going through the spinning process of fiber pretreatment → blending → opening and dust removal → carding → drawing → roving → fine spinning → winding → warping → sizing → warp threading → weaving.

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