Preparation method of long-acting heat-storage warm-keeping antibacterial lyocell fiber

Abstract

The invention discloses a preparation method of long-acting heat-storage warm-keeping antibacterial lyocell fibers, and belongs to the technical field of regenerated cellulose fibers. The preparation method of the lyocell fiber comprises the following steps: step SS1: stirring, mixing and dissolving cellulose pulp, an NMMO organic solvent, zirconium carbide micro powder and nano biochar according to a certain mass ratio at a certain temperature, and then defoaming and filtering to obtain a homogeneous phase mixed spinning solution with the fiber forming solid content concentration of 8%; and step SS2, spraying the obtained mixed spinning solution in air through a spray head, immersing the mixed spinning solution in a low-concentration NMMO aqueous solution for solidification forming, and then drafting, washing, cutting, washing, oiling and drying to obtain the finished fiber. The temperature rise speed of the heat-storage warm-keeping cellulose fiber fabric is far higher than that of a conventional lyocell fiber fabric, the temperature difference can reach 13.5 DEG C when a light source irradiates for 10 min, it is indicated that light energy can be effectively converted into heat energy in the presence of zirconium carbide in fibers, and the good warm-keeping effect is achieved.

Description

Technical Field

[0001] The invention relates to a method for preparing long-acting heat-storing, warm-keeping and antibacterial lyocell fiber, belonging to the technical field of regenerated cellulose fiber. Background Art

[0002] Lyocell fiber, commonly known as "Tencel Velvet", is a biodegradable fiber made from natural and renewable cellulose-rich plants such as cotton linters, hemp, bamboo, and wood, which are removed from the raw materials, purified, and adjusted for molecular weight, and then physically dissolved and glued by dry-jet wet spinning using N-methylmorpholine oxide (NMMO) as a solvent. Compared with traditional cellulose fibers such as viscose fibers, the production process of Lyocell fiber is green and environmentally friendly, without any toxic or harmful chemical reactions, and the fiber has better mechanical properties. Lyocell fiber has many excellent properties of both natural and synthetic fibers, and can show good toughness in both dry and wet states. It has good hygroscopicity, good drape, easy dyeing, strong wear resistance, and high spinnability. It has the breathability and comfort of cotton, the strength of polyester, and the gloss and touch of silk. Lyocell fiber has a wide range of applications in clothing, industry, and other fields. It is known as the "green fiber of the 21st century" and the most valuable product in the history of man-made fibers over the past half century.

[0003] With people's unremitting pursuit of high-quality life, the development of healthy, comfortable, green, environmentally friendly, functional and personalized textiles has become the mainstream trend of the textile industry. Traditional thermal clothing is fluffy and bloated, which is not convenient for movement and lacks aesthetics. Its thermal insulation principle is mainly to prevent the heat emitted by the body from escaping. Lyocell fiber is high in strength, easy to dye, comfortable, breathable and cool, making it widely used in various fields such as clothing and bedding in the hot summer and autumn seasons. Similarly, the characteristics of close-fitting wear, breathable and cool also limit the company of Lyocell fiber in the cold season for people to keep warm, which greatly reduces the application of Lyocell fiber in the scene of keeping warm.

[0004] There are a large number of pathogens in the space and environment where people live. The immune system can protect the human body from pathogens when it is in a normal state. However, once the ecology is out of balance, pathogens will invade the human body and threaten human health through the digestive system, respiratory tract or skin. Textiles are an important medium for transmitting pathogens. The improvement of living standards has put forward higher requirements for the health care function of textiles. Therefore, the importance and demand for antibacterial and health-care lyocell fibers, as an important variety in the field of clothing fibers, are also increasing. Summary of the invention

[0005] The purpose of the present invention is to overcome the defects of the prior art, solve the above-mentioned technical problems, and provide a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber and a preparation method thereof.

[0006] First, the first purpose of the present invention is to provide a lyocell fiber product containing zirconium carbide particles, which can absorb visible light in sunlight, convert the absorbed light energy into heat energy, and reflect far infrared rays with a longer wavelength to warm the inside of the fiber product and its preparation method. Zirconium carbide can better absorb the energy of near infrared rays with a wavelength less than 2.0μm and convert it into heat energy. It has a good absorption capacity for sunlight in the range of 0.3-2μm, which accounts for 95% of sunlight, so it can effectively absorb and store external energy. The infrared heat radiation wavelength emitted by the human body is about 10μm, and zirconium carbide has a reflective property for infrared rays with a wavelength greater than 2μm. Therefore, when people wear clothes containing zirconium carbide, the infrared rays of the human body are not easy to radiate outward, thereby playing a good warming effect.

[0007] Secondly, the second purpose of the present invention is that the prepared lyocell fiber has the effect of light-induced heat storage and warmth preservation, and because the plant-derived biochar antibacterial component is evenly distributed in the fiber, the fiber also has the effect of permanent antibacterial health care. The plant-derived biochar antibacterial heat storage and warmth preservation lyocell fiber, the biochar antibacterial component is made of peach tree as raw material, which is crushed into peach sawdust, and then the peach sawdust is decomposed into biochar in a low-oxygen and high-temperature environment. The biochar material is a porous irregular sheet-like nano material with strong adsorption and positive charge on the surface. It combines with the specific part of the bacterial cell membrane or the viral envelope, causing the membrane permeability and charge distribution to be changed, resulting in cell death or virus inactivation, and achieving antibacterial effect on fungi, bacteria and viruses.

[0008] The present invention specifically adopts the following technical scheme: a method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber, comprising the following steps:

[0009] Step SS1: mixing and dissolving cellulose pulp, NMMO organic solvent, zirconium carbide powder and nano-biochar in a certain mass ratio at a certain temperature, and then degassing and filtering to obtain a homogeneous mixed spinning solution with a fiber solid content concentration of 8%;

[0010] Step SS2: The mixed spinning solution obtained in the above step SS1 is sprayed out from a nozzle in the air, passed through an air bath, and then immersed in a low concentration NMMO aqueous solution for coagulation and formation, and then drawn, washed, cut, washed, oiled and dried to obtain the finished fiber.

[0011] As a preferred embodiment, the biochar antibacterial agent is a non-food single-component material, a bio-based flexible carbon nanomaterial, and does not contain any heavy metals. It is high temperature resistant and can inhibit bacteria, molds and viruses at the same time.

[0012] As a preferred embodiment, the cellulose pulp includes but is not limited to at least one of wood pulp, bamboo pulp, hemp pulp, straw pulp and cotton pulp.

[0013] As a preferred embodiment, the degree of polymerization of the cellulose pulp is 300-1600.

[0014] As a preferred embodiment, the cellulose pulp includes wood pulp and / or bamboo pulp.

[0015] As a preferred embodiment, the wood pulp includes coniferous wood pulp and / or hardwood wood pulp.

[0016] As a preferred embodiment, the spinning solution in step SS1 includes the following components in percentage by mass: 8-15% cellulose pulp, 74.5-78.5% NMMO organic solvent, 0.01-4.0% zirconium carbide powder, 0.01-1% biochar, and the remainder is water.

[0017] As a preferred embodiment, the particle size of the zirconium carbide powder is 0.1-0.5 μm, and the content in the fiber spinning solution is preferably 0.05-3.0%; the particle size of the nano biochar is 100-800 nm, and the content in the fiber spinning solution is preferably 0.05-0.8%. The particle size in the present invention refers to the average diameter of the particles.

[0018] As a preferred embodiment, the particle size of the zirconium carbide powder is 0.4 μm.

[0019] As a preferred embodiment, the dissolution temperature of the mixed dissolution in step SS1 is 80-110° C., and the dissolution time is 10-240 min.

[0020] As a preferred embodiment, the oiling temperature in step SS2 is 45-80° C., and the oiling time is 2-8 min.

[0021] The beneficial effects achieved by the present invention are as follows: first, according to the light absorption and heat preservation test method (BQE A036-2011), a light source simulating sunlight is used to irradiate the test sample under the same environment, and the surface temperature change is observed after a period of time, and the present invention is compared with a conventional fiber sample. Under the irradiation of the same light source, after the same time, the temperature rise rate of the heat-storing and warm-keeping Lyocell cellulose fiber fabric is much higher than that of the conventional Lyocell fiber fabric. When the light source is irradiated for 10 minutes, the temperature difference can reach 13.5°C, indicating that the presence of zirconium carbide in the fiber can effectively convert light energy into heat energy and achieve a good warming effect; second, in terms of antibacterial, the antibacterial rate of the product of the present invention is ≥99% for Escherichia coli, ≥99% for Staphylococcus aureus, and ≥99% for Candida albicans (test standard GB / T 20944.2 adsorption method), the antibacterial rate of Aspergillus niger, Trichoderma viride, Penicillium funiculum, Chaetomium globosum and other molds is 0 level, and the detection standard is GB / T24346-2009 culture dish method; thirdly, the heat storage, warmth preservation and antibacterial dual-effect lyocell fiber raw material of the present invention is environmentally friendly and renewable, has good hygroscopicity, good heat storage and warmth preservation effect, wide antibacterial range and high degree, and the fabric prepared by it has a comfortable skin feel and can be used to make cold-proof clothing, thermal underwear, home leisure clothes, bedding and other cold-proof and warm textiles in cold seasons, and can also be widely used in clothing and textiles in various medical and health fields. DETAILED DESCRIPTION

[0022] The present invention is further described below. The following examples are only used to more clearly illustrate the technical solution of the present invention, and are not intended to limit the protection scope of the present invention.

[0023] Example 1

[0024] (1) Grinding cotton pulp with a degree of polymerization of 825 into 200-mesh fine powder, and then stirring and mixing the pulp fine powder, NMMO solvent, zirconium carbide powder with a particle size of 0.4 microns, and nano-biochar at a mass ratio of 9.8:115:0.2:0.08 at 100° C., and then degassing and filtering to obtain a homogeneous mixed spinning solution with a fiber solid content concentration of 8%;

[0025] (2) The mixed spinning solution obtained in the above step (1) is sprayed out from a nozzle in the air, passed through an air bath, and then put into a low concentration NMMO aqueous solution for coagulation and formation, and then drawn, washed, cut, washed, oiled and dried to obtain the finished fiber.

[0026] Results: dry breaking strength 3.44CN / dtex, wet breaking strength 2.23CN / dtex, wet modulus (5% BISA) 1.08CN / dtex, dry elongation 11.04%, powder content in fiber 1.85%, infrared normal emissivity (meaning: along the normal direction of the object interface, the object absorbs and emits infrared energy, its value ranges from 0 to 1. Generally speaking, the larger the value, the more heat is accumulated in the object) 83%, good spinnability. Fiber antibacterial rate Escherichia coli ≥99%, Staphylococcus aureus ≥99%, Candida albicans ≥99%, mold antibacterial level 0.

[0027] Example 2

[0028] (1) mixing wood pulp fines with a degree of polymerization of 596, NMMO solvent, zirconium carbide powder, and nano-biochar in a mass ratio of 9.6:90:0.4:0.04 at 98° C., stirring, mixing, and dissolving, and then degassing and filtering to obtain a mixed spinning solution with a fiber solid content concentration of 10%;

[0029] (2) The mixed spinning solution obtained in the above step (1) is sprayed into the air and then into a low concentration NMMO aqueous solution to coagulate and form, and then drawn, washed, cut, washed, oiled and dried to obtain the finished fiber.

[0030] Results: Dry breaking strength 3.29CN / dtex, wet breaking strength 2.17CN / dtex, wet modulus (5% BISA) 0.98CN / dtex, dry elongation 10.38%, powder content in fiber 3.75%, infrared phase emissivity 88%, excellent spinnability. Fiber antibacterial rate of large intestine ≥99%, golden Staphylococcus ≥99%, white niacin ≥99%, fungus antibacterial level 0.

[0031] Example 3

[0032] (1) mixing bamboo pulp powder with a degree of polymerization of 1200, NMMO solvent, zirconium carbide powder, and nano-biochar at a mass ratio of 9.4:190:0.6:0.02 at 98° C., stirring, mixing, and dissolving, and then degassing and filtering to obtain a mixed spinning solution with a fiber solid content concentration of 5%;

[0033] (2) The mixed spinning solution obtained in the above step (1) is sprayed out from a nozzle in the air, passed through an air bath, and then enters a low concentration NMMO aqueous solution to coagulate and form, and then is drawn, washed, cut, washed, oiled, and dried to obtain the finished fiber.

[0034] Results: Dry breaking strength 3.55CN / dtex, wet breaking strength 2.41CN / dtex, wet modulus (5% BISA) 1.13CN / dtex, dry elongation 9.48%, powder content in fiber 5.44%, infrared phase emissivity 88%, good spinnability. Fiber antibacterial rate of large intestine ≥99%, Staphylococcus aureus ≥99%, white niacin ≥99%, fungus antibacterial level 0.

[0035] Example 4

[0036] (1) Mix wood pulp fines with a degree of polymerization of 530, NMMO solvent, zirconium carbide powder and nano-biochar in a mass ratio of 9.9:73:0.1:0.1 at 95° C., stir, mix and dissolve, then degas and filter to obtain a mixed spinning solution with a fiber solid content concentration of 12%;

[0037] (2) The mixed spinning solution obtained in the above step (1) is sprayed out from a nozzle in the air and then enters into a low concentration NMMO aqueous solution to coagulate and form, and then is drawn, washed, cut, washed, oiled and dried to obtain the finished fiber.

[0038] Results: Dry breaking strength 3.10CN / dtex, wet breaking strength 2.08CN / dtex, wet modulus (5% BISA) 0.96CN / dtex, dry elongation 11.35%, powder content in fiber 0.95%, infrared phase emissivity 81%, excellent spinnability. Fiber antibacterial rate of large intestine ≥99%, golden Staphylococcus ≥99%, white niacin ≥99%, fungal antibacterial level 0.

[0039] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents. Any modification or equivalent replacement that does not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber, characterized in that: The steps include: Step SS1: mixing and dissolving cellulose pulp, NMMO organic solvent, zirconium carbide powder and nano-biochar in a certain mass ratio at a certain temperature, and then degassing and filtering to obtain a homogeneous mixed spinning solution with a fiber solid content concentration of 8%; Step SS2: The mixed spinning solution obtained in the above step SS1 is sprayed out from a nozzle in the air, passed through a short air bath, and then immersed in a low concentration NMMO aqueous solution for coagulation and formation, and then stretched, washed, cut, washed, oiled and dried to obtain the finished fiber.

2. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The cellulose pulp includes but is not limited to at least one of wood pulp, bamboo pulp, hemp pulp, straw pulp and cotton pulp.

3. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The polymerization degree of the cellulose pulp is 300-1600.

4. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The cellulose pulp includes wood pulp and / or bamboo pulp.

5. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 4, characterized in that: The wood pulp includes softwood pulp and / or hardwood pulp.

6. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The spinning solution in step SS1 comprises the following components in percentage by mass: 8-15% cellulose pulp, 74.5-78.5% NMMO organic solvent, 0.01-4.0% zirconium carbide powder, 0.01-1% biochar, and the balance is water.

7. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 4, characterized in that: The particle size of the zirconium carbide powder is 0.1-0.5 μm, and the content of the zirconium carbide powder in the fiber spinning solution is preferably 0.05-3.0%; the particle size of the nano biochar is 100-800 nm, and the content of the nano biochar powder in the fiber spinning solution is preferably 0.05-0.8%.

8. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 7, characterized in that: The particle size of the zirconium carbide powder is 0.4 μm.

9. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The dissolution temperature of the mixed dissolution in step SS1 is 80-110° C., and the dissolution time is 10-240 min.

10. The method for preparing a long-lasting heat-storing, warm-keeping and antibacterial lyocell fiber according to claim 1, characterized in that: The oiling temperature in step SS2 is 45-80° C., and the oiling time is 2-8 min.