CN111235659A - Lyocell fiber with heat storage and insulation functions and preparation method thereof - Google Patents
Lyocell fiber with heat storage and insulation functions and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
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Abstract
The invention discloses a lyocell fiber with heat storage and insulation functions and a preparation method thereof, the fiber is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution, and then spinning by utilizing the spinning solution, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene, the dispersing agent and the cotton pulp meal is 1: 0.1-0.2: 20-30. During preparation, graphene, a dispersing agent and cotton pulp are dissolved in an NMMO aqueous solution to prepare a spinning solution; and then spinning is carried out, and the obtained fiber is sequentially subjected to coagulating bath, alcohol washing, bleaching, water washing, oiling and drying to obtain the lyocell fiber with the heat storage and preservation functions. The strength performance of the composite material is close to that of lyocell fibers purchased in the market, and the composite material has a good heat storage function.
Description
Technical Field
The invention relates to the technical field of lyocell fibers, in particular to lyocell fibers with heat storage and preservation functions and a preparation method thereof.
Background
Along with the increasing living standard of people, various novel clothes are developed, wherein the clothes with the heat storage and heating functions are increasingly favored by people.
The lyocell fiber is a novel renewable cellulose fiber, and is prepared by directly dissolving spinning pulp by using N-methylmorpholine-N-oxide as a solvent and performing a spinning process. The lyocell fiber has the properties of hygroscopicity, dyeability, wearing comfort of natural fiber, high strength, durability and the like of synthetic fiber. The production process of the lyocell fiber has no pollution to the environment, can be naturally degraded, and is known as revolutionary fiber known as 21 century.
At present, the market demand of multifunctional textiles is increasingly strengthened, wherein, textiles with the functions of heat storage and heat preservation are increasingly popular with consumers, not only can play a role in keeping warm, but also play an important role in the aspect of attractive clothes. The Chinese patent application No. 200810244102.2 discloses a heat storage and insulation finishing method, which adopts a solution containing a heat storage and insulation composition to finish a fabric; the Chinese patent application No. 201010620582.5 discloses a lightweight heat-insulating fabric, which is prepared by adopting a hollow polyester fiber yarn with a hollow rate of 10-80% to imitate the heat-insulating concept of a thermos bottle. However, these methods are complicated and expensive, and their heat-insulating function is easily lost after long-term use.
Therefore, the urgent need to find a heat storage and insulation fiber with high efficiency, convenience, low cost and strong durability is a problem to be solved.
Disclosure of Invention
The invention provides a lyocell fiber with heat storage and preservation functions and a preparation method thereof. In the preparation process of the lyocell, wood pulp cellulose needs to be dissolved in a solvent; the graphene has heat storage and insulation properties under appropriate conditions, and the graphene is combined with the lyocell fibers to prepare the lyocell fibers containing the graphene, so that the lyocell fibers containing the graphene become heat storage and insulation fibers. However, since graphene is easily precipitated in a spinning solution for preparing lyocell fibers, the graphene is unevenly distributed in the spun lyocell fibers, and mixing thereof is difficult.
The technical scheme includes that the lyocell fiber with the heat storage and insulation functions is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution and then spinning the spinning solution to obtain the lyocell fiber, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene to the dispersing agent to the cotton pulp meal is 1: 0.1-0.2: 20-30.
Further, the solvent is an NMMO aqueous solution, and the concentration is 82-92 wt%.
Further, the mass concentration of the cotton pulp meal in the spinning solution is 12-15%.
Further, when the dispersing agent is prepared, firstly, dissolving acrylamide, diallyl dimethyl ammonium chloride and allyl polyoxyethylene ether in water to prepare a monomer solution, then, controlling the temperature to be 79-81 ℃ under the stirring condition, respectively dropwise adding the prepared monomer and an ammonium persulfate initiator into a container filled with water, and after dropwise adding, preserving heat for 3-4 hours to carry out reaction; and cooling to obtain dispersant solution, and finally dialyzing and spray drying to obtain dispersant powder.
Further, the mol ratio of the acrylamide to the diallyl dimethyl ammonium chloride to the allyl polyoxyethylene ether is 1: 0.3-0.5; the mass of the ammonium persulfate accounts for 0.1-2% of the total mass of the monomers.
Further, during dialysis treatment, the dispersing agent solution is placed into a dialysis bag with the molecular weight of 10000-20000, and is placed into deionized water with the volume of 1000 times for dialysis for 2-3 times, and the dialysis interval time is 24 hours.
The invention also relates to a method for preparing the lyocell fiber with the heat storage and preservation functions, which comprises the following steps:
1) preparing a spinning solution: dissolving graphene, a dispersing agent and cotton pulp into an NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 3-5 hours to prepare a spinning solution;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, then filtering, entering a spinning system for spinning, vertically stretching the sprayed silk yarns in the air, entering a coagulating bath, and coagulating and forming;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 85-92% for 3-5 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 12-16;
4) bleaching the fiber: immersing the fibers treated in the step 3) into a bleaching agent solution with the concentration of 0.1-0.3 g/L for 3-4 hours at the temperature of 50-55 ℃ at a bath ratio of 1: 24-28;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 3-4 hours at a bath ratio of 1: 20-25;
6) oiling the fibers: immersing the fibers treated in the step 5) into an oil bath solution of 3-4 g/L, wherein the oil bath temperature is 80-85 ℃, the time is 3-4 hours, and the bath ratio is 1: 15-20;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber with the functions of heat storage and heat preservation.
Further, grinding the graphene by adopting a ball mill to enable the particle size range of the graphene to be 200-500 nm; then, an aqueous NMMO solution was added and mixed.
Further, in the step 1), the initial concentration of the NMMO aqueous solution is 49-54%, the pressure reduction distillation is firstly carried out until the concentration is 95-98%, and then cotton pulp meal is added. The bath ratio of the mass of the pulp to the volume of the NMMO aqueous solution is 1: 12-16 g/mL.
Further, during spinning in the step 2), the length of an air gap of a spinning system is 7-9 cm, the spinning speed is 35-55 m/min, the aperture of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the solidification bath is filled with 10-14 wt% of NMMO aqueous solution, and the temperature is 0-14 ℃.
The invention has the following beneficial effects:
1. the dry breaking strength of the lyocell fiber with the heat storage and heat preservation functions is 50-52 cN/tex, the dry breaking elongation is 13-14%, the wet breaking strength of the fiber is 39-40 cN/tex, the wet breaking elongation is 17-19%, and the main strength performance of the lyocell fiber is superior to that of lyocell fibers purchased in the market. The cellulose fiber prepared by the invention is qualified lyocell fiber.
2. Aiming at the problem that graphene and lyocell fibers are difficult to uniformly combine, the invention prepares a dispersing agent which contains cationic groups and can be effectively adsorbed on the surface of graphene; the polyoxyethylene can form a long-chain branch to generate strong dispersing performance, so that the graphene is well and uniformly distributed in the spinning solution, and the uniform distribution of the graphene in the lyocell fibers is realized. The prepared lyocell fabric with the heat storage and insulation functions is worn on a human body, and has a good heat storage function.
3. According to the invention, NMMO is adopted to simultaneously dissolve cellulose and nano graphene, and then the cellulose and the nano graphene are spun to prepare lyocell fibers with heat storage and preservation functions; the lyocell fiber with the heat storage and preservation functions prepared by the method has the advantages of simple production process, low price and small environmental pollution in the production process.
Drawings
FIG. 1 is an electron micrograph of lyocell fiber a prepared in example 1.
Detailed Description
The invention will be further elucidated with reference to the following examples.
Preparation of the dispersant:
simultaneously dissolving acrylamide, diallyl dimethyl ammonium chloride and allyl polyoxyethylene ether (n ═ 23) in 150mL of deionized water to prepare a monomer solution for later use; wherein the mol ratio of the acrylamide to the diallyl dimethyl ammonium chloride to the allyl polyoxyethylene ether is 1: 0.5; then, under the stirring condition, controlling the temperature to be 79-81 ℃, respectively dropwise adding the prepared monomer and an ammonium persulfate initiator into a four-neck flask filled with 250mL of deionized water, wherein the mass of the ammonium persulfate accounts for 1% of the total mass of the monomer, the dropwise adding time is controlled to be 3h, and after the dropwise adding is finished, keeping the temperature for 4 h; and finally, cooling to obtain a dispersant solution, putting the dispersant solution into a dialysis bag with the molecular weight of 10000-20000, putting the dialysis bag into deionized water with the volume of 1000 times of the dialysis bag for dialysis for 3 times, wherein the dialysis time interval is 24 hours, and then, spray-drying the solvent in the dialysis bag to obtain the powdery dispersant.
Example 1:
a lyocell fiber with heat storage and heat preservation functions is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution, and then spinning by utilizing the spinning solution to prepare the lyocell fiber, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene, the dispersing agent and the cotton pulp meal is 1: 0.1: 20.
The preparation method comprises the following steps:
1) preparing a spinning solution: grinding the purchased graphene by using a ball mill to enable the particle size range of the purchased graphene to be 200-500 nm; distilling 49% by mass of NMMO aqueous solution under reduced pressure to 92% by mass of NMMO aqueous solution, dissolving graphene, a dispersing agent and cotton pulp meal in the NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 3 hours to prepare 12% by mass of uniform spinning solution;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, filtering, and entering a spinning system, wherein the length of an air gap is 7-9 cm, the spinning speed is 35-55 m/min, the pore diameter of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 14 percent of NMMO aqueous solution, and the temperature of the coagulating bath is 0-14 ℃;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 92% for 5 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 16;
4) bleaching the fiber: immersing the fiber treated in the step 3) into a bleaching agent solution (name: strong chlorine essence, produced by Shandong Jia clean water treatment science and technology Limited), the immersion time is 4 hours, the solution temperature is 50-55 ℃, and the bath ratio is 1: 28;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 3 hours at a bath ratio of 1: 20;
6) oiling the fibers: immersing the fiber treated in the step 5) into 3g/L of oil bath solution (model: HY-101, produced by Hangzhou Huaya chemical Co., Ltd.), and oil bath at 80-85 deg.C for 3 hr at a bath ratio of 1: 20;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber a with the functions of heat storage and heat preservation, wherein an electron microscope image of the lyocell fiber a is shown in figure 1.
Example 2:
a lyocell fiber with heat storage and heat preservation functions is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution, and then spinning by utilizing the spinning solution to prepare the lyocell fiber, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene, the dispersing agent and the cotton pulp meal is 1: 0.15: 25.
The preparation method comprises the following steps:
1) preparing a spinning solution: grinding the purchased graphene by using a ball mill to enable the particle size range of the purchased graphene to be 200-500 nm; dissolving graphene, a dispersing agent and cotton pulp into an NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 3 hours to prepare a uniform spinning solution with the mass fraction of 13%;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, filtering, and entering a spinning system, wherein the length of an air gap is 7-9 cm, the spinning speed is 35-55 m/min, the pore diameter of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 12 percent of NMMO aqueous solution, and the temperature of the coagulating bath is 0-14 ℃;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 88% for 3-5 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 14;
4) bleaching the fiber: immersing the fiber treated in the step 3) into a bleaching agent solution (name: strong chlorine essence, produced by Shandong Jia clean water treatment science and technology Limited), the immersion time is 3 hours, the solution temperature is 50-55 ℃, and the bath ratio is 1: 26;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 4 hours at a bath ratio of 1: 22;
6) oiling the fibers: the fiber treated in step 5) was immersed in 3.5g/L of an oil bath solution (type: HY-101, produced by Hangzhou Huaya chemical Co., Ltd.), and oil bath at 80-85 deg.C for 3 hr at a bath ratio of 1: 18;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber b with the functions of heat storage and heat preservation.
Example 3:
a lyocell fiber with heat storage and heat preservation functions is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution, and then spinning by utilizing the spinning solution to prepare the lyocell fiber, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene, the dispersing agent and the cotton pulp meal is 1: 0.2: 30.
The preparation method comprises the following steps:
1) preparing a spinning solution: grinding the purchased graphene by using a ball mill to enable the particle size range of the purchased graphene to be 200-500 nm; distilling an NMMO aqueous solution with the mass fraction of 54% to an NMMO aqueous solution with the mass fraction of 83%, dissolving graphene, a dispersing agent and cotton pulp into the NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 5 hours to prepare a uniform spinning solution with the mass fraction of 15%;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, filtering, and entering a spinning system, wherein the length of an air gap is 7-9 cm, the spinning speed is 35-55 m/min, the pore diameter of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 11 percent of NMMO aqueous solution, and the temperature of the coagulating bath is 0-14 ℃;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 85-92% for 3 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 12;
4) bleaching the fiber: immersing the fiber treated in the step 3) into a bleaching agent solution (name: strong chlorine essence, produced by Shandong Jia clean water treatment science and technology Limited), the immersion time is 3 hours, the solution temperature is 50-55 ℃, and the bath ratio is 1: 24;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 3 hours at a bath ratio of 1: 21;
6) oiling the fibers: immersing the fiber treated in the step 5) into 4g/L of oil bath solution (model: HY-101, produced by Hangzhou Huaya chemical Co., Ltd.), and oil bath temperature of 80-85 deg.C for 4 hr at bath ratio of 1: 15;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber c with the functions of heat storage and heat preservation.
Comparative example 1:
the lyocell fiber with the heat storage and insulation functions is prepared by mixing graphene and lyocell fiber raw materials with a solvent to prepare a spinning solution and then spinning by utilizing the spinning solution, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene to the cotton pulp meal is 1: 25.
The preparation method comprises the following steps:
1) preparing a spinning solution: grinding the purchased graphene by using a ball mill to enable the particle size range of the purchased graphene to be 200-500 nm; dissolving graphene and cotton pulp meal in an NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 3 hours to prepare a uniform spinning solution with the mass fraction of 13%;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, filtering, and entering a spinning system, wherein the length of an air gap is 7-9 cm, the spinning speed is 35-55 m/min, the pore diameter of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the sprayed silk threads are vertically stretched in the air, enter a coagulating bath, and are coagulated and formed, wherein the concentration of the coagulating bath is 12 percent of NMMO aqueous solution, and the temperature of the coagulating bath is 0-14 ℃;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 88% for 3-5 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 14;
4) bleaching the fiber: immersing the fiber treated in the step 3) into a bleaching agent solution (name: strong chlorine essence, produced by Shandong Jia clean water treatment science and technology Limited), the immersion time is 3 hours, the solution temperature is 50-55 ℃, and the bath ratio is 1: 26;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 4 hours at a bath ratio of 1: 22;
6) oiling the fibers: the fiber treated in step 5) was immersed in 3.5g/L of an oil bath solution (type: HY-101, produced by Hangzhou Huaya chemical Co., Ltd.), and oil bath at 80-85 deg.C for 3 hr at a bath ratio of 1: 18;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber d with the functions of heat storage and heat preservation.
The thermal storage and insulation performance of the lyocell fibers a, b, c and d with the thermal storage and insulation functions prepared in the above specific examples 1-3 and comparative example 1 of the present invention is tested for strength, and the test method refers to GB/T-24218.3-2010 test method for textile and non-woven fabrics part 3: determination of breaking strength and breaking elongation, a FAVIMAT-BOBOBOT 2 full-automatic single fiber universal tester is adopted to determine the strength performance of the test samples, no less than 30 test samples are tested, and the test average value is taken. The test results are shown in table 1, wherein the lyocell fibers with the heat storage and preservation functions a, b, c and d are abbreviated as follows: fibers a, b, c and d, lyocell fibers available from Shandong Mimex textile technology, Inc.
TABLE 1 mechanical Properties of fibers a, b, c, d and of the lyocell fibers purchased
| Item | Fiber a | Fiber b | Fiber c | Fibre d | Purchased lyocell fibre |
| Dry breaking Strength (cN/tex) | 50.4 | 51.6 | 51.1 | 50.1 | 48.5 |
| Elongation at Dry Break (%) | 13.3 | 13.7 | 13.3 | 11.3 | 11.4 |
| Wet tensile Strength (cN/tex) | 39.7 | 39.2 | 39.3 | 36.9 | 36.3 |
| Wet elongation at break (%) | 17.3 | 17.5 | 18.2 | 16.2 | 15.7 |
As can be seen from Table 1, the dry breaking strength of the lyocell fibers with the heat storage and heat preservation functions prepared in the embodiments 1 to 3 is between 50 and 52cN/tex, which is slightly higher than that of the purchased lyocell fibers; the dry breaking elongation of the composite material is between 13 and 14 percent and is slightly higher than that of purchased lyocell fiber; the wet breaking strength of the fiber is between 39 and 40cN/tex, which is slightly higher than that of the purchased lyocell fiber, and the wet breaking elongation of the fiber is between 17 and 19 percent, which is slightly higher than that of the purchased lyocell fiber. From the test result of the mechanical property, the thermal storage and insulation function lyocell fibers prepared in the embodiments 1 to 3 have the mechanical property superior to that of purchased lyocell fibers, and therefore, the cellulose fibers prepared by the method are qualified lyocell fibers. The thermal storage and insulation function lyocell fiber prepared in the comparative example 1 has slightly poorer mechanical properties than those of the thermal storage and insulation function lyocell fibers prepared in the examples 1 to 3, but is close to the mechanical properties of lyocell fibers in the market.
The thermal insulation performance test is carried out on the lyocell fibers a, b, c and d with the thermal storage and thermal insulation functions prepared in the specific examples 1-3 and the comparative example 1, the prepared lyocell fibers a, b, c and d and purchased lyocell fibers are spun into fabrics to meet the test requirements, the thermal insulation Crohn value is tested by adopting a JIS L1096KES thermal insulation tester, the thermal insulation effect can be reflected by the thermal insulation Crohn value, and the test results are shown in Table 2.
TABLE 2 insulation Properties of fibers a, b, c, d and of the lyocell fibers purchased
| Item | Fiber a | Fiber b | Fiber c | Fibre d | Purchased lyocell fibre |
| Thermal insulating clo value | 0.75 | 0.74 | 0.77 | 0.53 | 0.41 |
Generally, a higher insulating Kraft value indicates a better insulating property of the fabric. As can be seen from Table 2, the insulation Crohn values of the fibers a, b and c prepared in the examples 1-3 are more than 0.74, the insulation Crohn value of the fiber d prepared in the comparative example 1 is only 0.53, and the insulation Crohn values are obviously inferior to the fibers a, b and c prepared in the examples 1-3, which shows that the prepared dispersant plays an important role in insulation performance. In general, the lyocell fibers a, b, c and d with the heat storage and heat preservation functions prepared in the embodiments 1 to 3 and the comparative example 1 are superior to the purchased lyocell fibers in heat preservation performance.
Claims (10)
1. A lyocell fiber with heat storage and insulation functions is characterized in that:
the fiber is prepared by mixing graphene, a dispersing agent, lyocell fiber raw materials and a solvent to prepare a spinning solution, and then spinning by utilizing the spinning solution, wherein the lyocell fiber raw materials are cotton pulp meal, and the mass ratio of the graphene, the dispersing agent and the cotton pulp meal is 1: 0.1-0.2: 20-30.
2. The lyocell fiber having a thermal storage and insulation function according to claim 1, wherein: the solvent is an NMMO aqueous solution, and the concentration is 82-92 wt%.
3. The lyocell fiber having a thermal storage and insulation function according to claim 2, wherein: wherein the mass concentration of the cotton pulp meal in the spinning solution is 12-15%.
4. The lyocell fiber having a thermal storage and insulation function according to claim 1, wherein: when the dispersing agent is prepared, firstly, dissolving acrylamide, diallyl dimethyl ammonium chloride and allyl polyoxyethylene ether in water to prepare a monomer solution, then controlling the temperature to be 79-81 ℃ under the stirring condition, respectively dropwise adding the prepared monomer and an ammonium persulfate initiator into a container filled with water, and after dropwise adding, preserving heat for 3-4 hours to carry out reaction; and cooling to obtain dispersant solution, and finally dialyzing and spray drying to obtain dispersant powder.
5. The lyocell fiber having a thermal storage and insulation function according to claim 4, wherein: the mol ratio of the acrylamide to the diallyl dimethyl ammonium chloride to the allyl polyoxyethylene ether is 1: 0.3-0.5; the mass of the ammonium persulfate accounts for 0.1-2% of the total mass of the monomers.
6. The lyocell fiber having a thermal storage and insulation function according to claim 4, wherein: during dialysis treatment, the dispersant solution is placed into a dialysis bag with the molecular weight of 10000-20000, and is placed into deionized water with the volume of 1000 times for dialysis for 2-3 times, and the dialysis interval time is 24 hours.
7. The method for preparing the lyocell fiber having the heat-accumulating and heat-preserving function according to any one of claims 1 to 6, comprising the steps of:
1) preparing a spinning solution: dissolving graphene, a dispersing agent and cotton pulp into an NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-130 ℃ in vacuum for 3-5 hours to prepare a spinning solution;
2) spinning of lyocell fibers: adding the spinning solution into a screw extruder, further dissolving at 96-115 ℃, then filtering, entering a spinning system for spinning, vertically stretching the sprayed silk yarns in the air, entering a coagulating bath, and coagulating and forming;
3) alcohol washing of the fibers: immersing the fiber treated in the step 2) into an ethanol solution with the concentration of 85-92% for 3-5 hours, wherein the solution temperature is room temperature, and the bath ratio is 1: 12-16;
4) bleaching the fiber: immersing the fibers treated in the step 3) into a bleaching agent solution with the concentration of 0.1-0.3 g/L for 3-4 hours at the temperature of 50-55 ℃ at a bath ratio of 1: 24-28;
5) and (3) water washing of the fiber: immersing the fibers treated in the step 4) into hot water at the temperature of 70-85 ℃ for 3-4 hours at a bath ratio of 1: 20-25;
6) oiling the fibers: immersing the fibers treated in the step 5) into an oil bath solution of 3-4 g/L, wherein the oil bath temperature is 80-85 ℃, the time is 3-4 hours, and the bath ratio is 1: 15-20;
7) drying the fibers: drying the fiber treated in the step 6) to obtain the lyocell fiber with the functions of heat storage and heat preservation.
8. The method of claim 7, wherein: firstly, grinding graphene by adopting a ball mill to enable the particle size range of the graphene to be 200-500 nm; then, an aqueous NMMO solution was added and mixed.
9. The method of claim 7, wherein: in the step 1), the initial concentration of the NMMO aqueous solution is 49-54%, reduced pressure distillation is firstly carried out until the concentration is 95-98%, and then cotton pulp meal is added.
10. The method of claim 7, wherein: step 2) during spinning, the length of an air gap of a spinning system is 7-9 cm, the spinning speed is 35-55 m/min, the aperture of a spinneret plate is 15-115 mu m, and the length of a pore capillary is 350-800 mu m; the solidification bath is filled with 10-14 wt% of NMMO aqueous solution, and the temperature is 0-14 ℃.
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Cited By (2)
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|---|---|---|---|---|
| CN112030269A (en) * | 2020-09-04 | 2020-12-04 | 安徽瑜合警用装备有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
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