CN111334880B - Photochromic lyocell fibers and method for making same - Google Patents
Photochromic lyocell fibers and method for making same 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The invention discloses photochromic lyocell fiber and a preparation method thereof, wherein the photochromic lyocell fiber is prepared by mixing photochromic raw materials into lyocell fiber raw material spinning solution for spinning; the mass ratio of the photochromic raw material to the lyocell fiber raw material is 1: 25-35; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp meal. The fiber has good photochromic characteristic and stable performance, and the preparation method of the fiber is simple and has low cost.
Description
Technical Field
The invention relates to the technical field of lyocell fibers, in particular to photochromic lyocell fibers and a preparation method thereof.
Background
Currently, with the increasing living standard of people, various clothes with special properties are developed, such as: antibacterial, waterproof, wrinkle-resistant, antistatic, etc. Among these garments, photochromic functional garments are popular among people, particularly in the fields of magic artists, camouflage in the military, apparel for children, and the like. With the rapid development of photochromic materials, the rapid development of photochromic clothes is driven.
Lyocell, as a new type of renewable cellulose fiber, has many advantages, such as: short production period, little environmental pollution, easy degradation after use, easy dyeing, good hand feeling, skin affinity, high mechanical strength, durability and the like, thus being praised as one of 21 novel fibers with most development potential. Lyocell fibers are used in various textile materials due to their excellent properties, such as: the chinese patent application No. 201810758129.7 reports an antibacterial textile material containing a large amount of lyocell fibers; chinese patent application No. 201711186225.0 reports a close-fitting, warm-keeping and comfortable cheongsam that also contains a large amount of lyocell fibers. Literature investigations have shown that lyocell fibres are of great interest.
The main component of the lyocell fiber is cellulose, if the cellulose is directly combined with the photochromic monomer, the combination force of the cellulose and the photochromic monomer is weak, and the photochromic monomer can fall off after being washed for many times, thereby influencing the photochromic performance of the lyocell fiber. Therefore, finding an effective way to achieve a strong bond between lyocell fibers and photochromic monomers is a difficult point to overcome in preparing excellent photochromic lyocell fibers.
Disclosure of Invention
The invention provides photochromic lyocell fiber and a preparation method thereof, and the fiber has good photochromic characteristic, stable performance, simple fiber preparation method and low cost.
The technical scheme of the invention is that the photochromic lyocell fiber is prepared by mixing photochromic raw materials into a lyocell fiber raw material spinning solution for spinning; the mass ratio of the photochromic raw material to the lyocell fiber raw material is 1: 25-35; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp meal.
In a preferable scheme, the mass ratio of the photochromic raw material to the lyocell fiber raw material is 1: 28-30.
Furthermore, in the spinning solution, the solvent is NMMO, and the mass concentration of the spinning solution prepared finally is 12-15%.
In a more preferable scheme, the preparation method of the modified photochromic lignin comprises the following steps: dissolving sodium lignosulfonate in water, dissolving 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone in N, N-dimethylformamide, dissolving ammonium persulfate in water to prepare an ammonium persulfate aqueous solution, respectively and simultaneously dropwise adding the N, N-dimethylformamide and the ammonium persulfate aqueous solution in which the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone are dissolved into the sodium lignosulfonate aqueous solution, preserving heat for 2-3 hours after dropwise adding is finished, and controlling the reaction temperature to be 70-80; and (3) distilling the solution under reduced pressure after the reaction is finished to obtain a solid precipitate, namely the modified photochromic lignin.
The involved reaction formula is as follows:
furthermore, the mass ratio of the sodium lignosulfonate to the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone and the ammonium persulfate is 10-12:1: 2-5.
The invention also relates to a process for preparing the photochromic lyocell fibre, comprising the steps of:
1) preparing a spinning solution: dissolving photochromic raw materials 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) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at the temperature of 70-85 ℃ for washing, wherein the washing time is 3-5 minutes, and the bath ratio is 1: 20-25;
4) oiling the fibers: immersing the fibers treated in the step 3) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 3-5 minutes, and the bath ratio is 1: 15-20;
5) drying the fibers: and (3) drying the fiber treated in the step 4) to obtain the photochromic lyocell fiber.
Further, 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 reaches 95-98%, and then photochromic raw materials and cotton pulp meal are added.
Further, the mass concentration of the spinning solution obtained in the step 1) is 12-15%.
Further, in the step 2), during spinning, the length of an air gap in 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 capillary tube is 350-800 mu m.
Further, in the step 2), the temperature of the coagulation bath is 0-14 ℃ when the concentration of the NMMO aqueous solution in the coagulation bath is 10-14%.
The invention has the following beneficial effects:
1. the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone has photochromic performance, but the solubility of the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone in NMMO is poor.
2. The modified photochromic lignin and the lyocell cellulose have strong binding capacity, the photochromic lyocell fiber prepared by the method has the photochromic performance which is not weakened after being washed for many times, and the raw materials adopted during the preparation process have wide sources, low price, small pollution to the environment during the production process, and better application and popularization prospects.
3. The photochromic lyocell fiber prepared by the method has the dry breaking strength of 49-50 cN/tex, the dry breaking elongation of 16-18%, the wet breaking strength of 37-38 cN/tex and the wet breaking elongation of 15-16%. From the test result of mechanical property, the mechanical property of the photochromic lyocell fiber is superior to that of the common lyocell fiber after the modified photochromic lignin is added.
Detailed Description
The invention will be further elucidated with reference to the following examples.
The specific preparation method of the modified photochromic lignin comprises the following steps:
dissolving 2kg of sodium lignosulfonate in 30L of deionized water, dissolving 0.1kg of 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone in 30L N, N-dimethylformamide, dissolving 0.2-0.5 kg of ammonium persulfate in 30L of deionized water to prepare an ammonium persulfate aqueous solution, respectively and simultaneously dropwise adding the N, N-dimethylformamide dissolved with the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone and the ammonium persulfate aqueous solution to the sodium lignosulfonate aqueous solution, preserving heat for 2-3 hours after dropwise adding is finished, and controlling the reaction temperature to be 70-80. And (3) distilling the solution under reduced pressure after the reaction is finished to obtain a solid precipitate, namely the modified photochromic lignin.
Example 1:
photochromic lyocell fiber is prepared by mixing photochromic raw materials into a lyocell fiber raw material spinning solution for spinning; the mass ratio of photochromic raw material to lyocell fiber raw material is 1: 30; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp meal.
The preparation method comprises the following steps:
(1) preparing a spinning solution: and distilling 49% by mass of NMMO aqueous solution under reduced pressure to 96% by mass of NMMO aqueous solution, dissolving the modified photochromic lignin and cotton pulp meal in the NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 125-130 ℃ in vacuum for 3 hours to prepare a uniform spinning solution with 13% by mass. Wherein the mass ratio of the modified photochromic lignin to the cotton pulp meal is 1: 30.
(2) Spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 96-115 ℃, then filtering, and entering a spinning system, wherein the main parameters of the spinning system are controlled as follows: the length of the air gap is 7-9 cm, the spinning speed is 35-55 m/min, the aperture of the spinneret plate is 15-115 mu m, and the length of the capillary tube is 350-800 mu m. And (3) vertically stretching the sprayed silk in the air, feeding the silk into a coagulating bath, and coagulating and forming, wherein the coagulating bath is an NMMO (N-methyl-amino-methyl-N-methyl-MO) aqueous solution with the mass concentration of 10-14%, and the temperature of the coagulating bath is 0-14 ℃.
(3) And (3) water washing of the fiber: immersing the fiber treated in the step (2) into hot water at the temperature of 70-85 ℃ for 3-5 minutes at a bath ratio of 1: 20-25.
(4) Oiling the fibers: and (3) immersing the fibers treated in the step (3) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 3-5 minutes, and the bath ratio is 1: 15-20.
(5) Drying the fibers: and (4) drying the fiber treated in the step (4) to obtain the photochromic lyocell fiber a.
Example 2:
photochromic lyocell fiber is prepared by mixing photochromic raw materials into a lyocell fiber raw material spinning solution for spinning; the mass ratio of photochromic raw material to lyocell fiber raw material is 1: 25; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp meal.
The preparation method comprises the following steps:
(1) preparing a spinning solution: distilling the NMMO aqueous solution with the mass fraction of 50% to the NMMO aqueous solution with the mass fraction of 98%, dissolving the modified photochromic lignin and cotton pulp meal in the NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 115-120 ℃ in vacuum for 3 hours to prepare the uniform spinning solution with the mass fraction of 12%. Wherein the mass ratio of the modified photochromic lignin to the cotton pulp meal is 1: 25.
(2) Spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 96-115 ℃, then 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 coagulating bath is an NMMO (N-methyl-MO) aqueous solution with the concentration of 10-14%, and the temperature of the coagulating bath is 0-14 ℃.
(3) And (3) water washing of the fiber: immersing the fiber treated in the step (2) into hot water at the temperature of 70-85 ℃ for 3-5 minutes at a bath ratio of 1: 20-25.
(4) Oiling the fibers: and (3) immersing the fibers treated in the step (3) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 3-5 minutes, and the bath ratio is 1: 15-20.
(5) Drying the fibers: and (4) drying the fiber treated in the step (4) to obtain the photochromic lyocell fiber b.
Example 3:
photochromic lyocell fiber is prepared by mixing photochromic raw materials into a lyocell fiber raw material spinning solution for spinning; the mass ratio of photochromic raw material to lyocell fiber raw material is 1: 35; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp meal.
The preparation method comprises the following steps:
(1) preparing a spinning solution: and distilling the NMMO aqueous solution with the mass fraction of 53% to the NMMO aqueous solution with the mass fraction of 95%, dissolving photochromic organic matter modified photochromic lignin and cotton pulp meal in the NMMO aqueous solution, and stirring and dissolving in a reaction kettle at 120-130 ℃ for 4 hours in vacuum to prepare the uniform spinning solution with the mass fraction of 15%. Wherein the mass ratio of the modified photochromic lignin to the cotton pulp meal is 1: 35.
(2) Spinning of lyocell fibers: adding the spinning solution treated in the step (1) into a screw extruder, further dissolving at 96-115 ℃, then 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; and (3) vertically stretching the sprayed silk in the air, feeding the silk into a coagulating bath, and coagulating and forming, wherein the coagulating bath is an NMMO (N-methyl-amino-methyl-N-methyl-MO) aqueous solution with the mass concentration of 10-14%, and the temperature of the coagulating bath is 0-14 ℃.
(3) And (3) water washing of the fiber: immersing the fiber treated in the step (2) into hot water at the temperature of 70-85 ℃ for 3-5 minutes at a bath ratio of 1: 20-25.
(4) Oiling the fibers: and (3) immersing the fibers treated in the step (3) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 3-5 minutes, and the bath ratio is 1: 15-20.
(5) Drying the fibers: and (4) drying the fiber treated in the step (4) to obtain the photochromic lyocell fiber c.
The photochromic lyocell fibers obtained in examples 1 to 3 were evaluated for their properties.
(1) Photochromic performance test: photochromic lyocell fibers a, b and c prepared in the above specific examples 1 to 3 were subjected to photochromic performance test. The light source was irradiated with a 500W xenon lamp for 5 minutes, and the photochromic lyocell fibers a, b and c changed from natural (white) to blue. The photochromic lyocell fibers a, b and c were subjected to standard washing 20 times and photochromic performance test again, and as a result, it was found that the photochromic lyocell fibers a, b and c had the same photochromic performance as before washing.
(2) Testing the mechanical properties of the fibers: the photochromic lyocell fibers a, b and c prepared in the above specific embodiments 1 to 3 are subjected to a strength performance test, and the test method refers to GB/T-24218.3-2010 "test method for textile and non-woven fabric 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 photochromic lyocell fibers a, b, c are abbreviated as fibers a, b, c and the lyocell fibers purchased from seohnd danau textile co.
TABLE 1 mechanical Properties of Ramie pulp Lyocell fibers a, b, c and of the purchased Lyocell fibers
As can be seen from Table 1, the dry breaking strength of the photochromic lyocell fibers is between 49 and 50cN/tex, which is slightly higher than that of the purchased lyocell fibers, and the dry breaking elongation of the photochromic lyocell fibers is between 16 and 18 percent, which is slightly higher than that of the purchased lyocell fibers; the wet breaking strength of the photochromic lyocell fiber is between 37 and 38cN/tex and is slightly higher than that of the purchased lyocell fiber, and the wet breaking elongation of the photochromic lyocell fiber is between 15 and 16 percent and is slightly higher than that of the purchased lyocell fiber. From the test result of mechanical property, the mechanical property of the photochromic lyocell fiber is superior to that of the purchased lyocell fiber, so that the photochromic lyocell fiber prepared by the method is qualified.
Claims (8)
1. A photochromic lyocell fiber characterized in that: the photochromic fabric is prepared by mixing photochromic raw materials into lyocell fiber raw material spinning solution for spinning; the mass ratio of the photochromic raw material to the lyocell fiber raw material is 1: 25-35; the photochromic raw material is modified photochromic lignin, and the lyocell fiber raw material is cotton pulp; the preparation method of the modified photochromic lignin comprises the following steps: dissolving sodium lignosulfonate in water, dissolving 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone in N, N-dimethylformamide, dissolving ammonium persulfate in water to prepare an ammonium persulfate aqueous solution, respectively and simultaneously dropwise adding the N, N-dimethylformamide and the ammonium persulfate aqueous solution in which the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone are dissolved into the sodium lignosulfonate aqueous solution, and keeping the temperature for 2-3 hours after dropwise adding, wherein the reaction temperature is controlled to be 70-80 ℃; after the reaction is finished, distilling the solution under reduced pressure to obtain a solid precipitate, namely the modified photochromic lignin; the mass ratio of the sodium lignosulfonate to the 6, 8-dichloro-3, 4-dihydro-1H-2-naphthalenone and the ammonium persulfate is 10-12:1: 2-5.
2. Photochromic lyocell fiber according to claim 1, characterized in that: the mass ratio of the photochromic raw material to the lyocell fiber raw material is 1: 28-30.
3. Photochromic lyocell fiber according to claim 1, characterized in that: in the spinning solution, the solvent is NMMO, and the mass concentration of the spinning solution prepared finally is 12-15%.
4. A process for preparing a photochromic lyocell fibre according to any one of claims 1 to 3, comprising the steps of:
1) preparing a spinning solution: dissolving photochromic raw materials 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) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at the temperature of 70-85 ℃ for washing, wherein the washing time is 3-5 minutes, and the bath ratio is 1: 20-25;
4) oiling the fibers: immersing the fibers treated in the step 3) into 3-4 g/L oil bath solution, wherein the oil bath temperature is 80-85 ℃, the time is 3-5 minutes, and the bath ratio is 1: 15-20;
5) drying the fibers: and (3) drying the fiber treated in the step 4) to obtain the photochromic lyocell fiber.
5. The method of claim 4, 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 photochromic raw materials and cotton pulp meal are added.
6. The method of claim 4, wherein: the mass concentration of the spinning solution obtained in the step 1) is 12-15%.
7. The method of claim 4, wherein: and 2) during spinning, in a spinning system, the length of an air gap 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.
8. The method of claim 4, wherein: in the step 2), the coagulating bath is an NMMO aqueous solution with the mass concentration of 10-14%, and the temperature of the coagulating bath is 0-14 ℃.
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| CN112323168A (en) * | 2020-11-25 | 2021-02-05 | 江苏杜为新材料科技有限公司 | Photochromic fiber and preparation method thereof |
| CN112760978A (en) * | 2021-02-01 | 2021-05-07 | 浙江松井纺织有限公司 | Improved processing technology of lyocell fiber |
| CN114775089A (en) * | 2022-05-18 | 2022-07-22 | 江苏金秋弹性织物有限公司 | Preparation method of photochromic elastic ribbon based on polyacid base |
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