CN112323168A - Photochromic fiber and preparation method thereof - Google Patents
Photochromic fiber and preparation method thereof Download PDFInfo
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- CN112323168A CN112323168A CN202011338086.0A CN202011338086A CN112323168A CN 112323168 A CN112323168 A CN 112323168A CN 202011338086 A CN202011338086 A CN 202011338086A CN 112323168 A CN112323168 A CN 112323168A
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- photochromic
- fiber
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The invention belongs to the technical field of preparation of polymer fibers, and discloses a photochromic fiber and a preparation method thereof. The fiber is prepared by mixing photochromic master batch into a polyethylene fiber or polypropylene fiber raw material spinning solution for spinning; the mass ratio of the photochromic master batch to the polyethylene fiber or polypropylene fiber raw material is 1: (30-40); the photochromic master batch is formed by mixing a photochromic agent and an auxiliary agent, and the photochromic agent comprises an inorganic photochromic agent and an organic photochromic agent. By using the organic photochromic agent, when visible light irradiates the fiber, the pigment of the fiber is lightened, and the light transmittance is increased, and when the visible light is reduced, the color of the fiber is darkened, and the light transmittance is reduced, so that the heat insulation performance of the fiber is ensured; the preparation method is simple and efficient, is suitable for large-scale production, and has good market application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation of polymer fibers, and particularly relates to a photochromic fiber and a preparation method thereof.
Background
Currently, with the increasing living standard of people, various fibers with special properties are developed, such as antibacterial, waterproof, wrinkle-resistant, antistatic, etc. Among these fibers, fibers having a photochromic function are popular among people, and are particularly used in the fields of magic artists, camouflage of military troops, clothes for children, and the like. With the rapid development of photochromic materials, the rapid development of photochromic fibers is driven.
In addition, although the fiber has the above special properties and excellent characteristics, there is still a certain limitation in use, that is, for example, in the textile field, the fabric is too thin and has poor shading performance, and if the fabric is too thick, the shading performance is too good, but the fabric affects light, especially absorbs too much light, and causes the fabric to generate heat, and the use is affected.
Therefore, how to develop a preparation method of photochromic fibers which have strong applicability and are suitable for being used as decorative materials becomes a problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a photochromic fiber, which changes color correspondingly through the reaction of the fiber to light, mainly changes different colors correspondingly through the reaction to ultraviolet light and visible light, not only has the function of ultraviolet resistance, but also can change the light transmittance of the fiber according to the irradiation of the visible light, and improves the applicability of the fiber.
In order to achieve the purpose, the invention adopts the following technical scheme:
the photochromic fiber is prepared by mixing photochromic master batch into a polyethylene fiber or polypropylene fiber raw material spinning solution for spinning; wherein the content of the first and second substances,
the mass ratio of the photochromic master batch to the polyethylene fiber or polypropylene fiber raw material is 1: (30-40), wherein the photochromic master batch is formed by mixing a photochromic agent and an auxiliary agent;
the photochromic agent is prepared from an inorganic photochromic agent and an organic photochromic agent according to a mass ratio of 1: 3, and mixing.
The photochromic fiber disclosed by the invention can change color along with the intensity of light, has good color fixing effect and thermal stability, can still show good color changing effect after long-term strong light irradiation, and has long service life, mild color and good eye fatigue resistance.
Preferably, the benign solvent of the spinning solution is NMMO, TFA or DCM, and the mass concentration of the spinning solution is 10-15%.
Preferably, the photochromic master batch is prepared by mixing a photochromic agent and an auxiliary agent, and the photochromic master batch comprises the following components in percentage by mass:
65-85% of photochromic agent,
15-30% of an auxiliary agent.
Further preferably, the auxiliary agent comprises one or more of an oxidant, a compatilizer, an aging inhibitor and a light stabilizer.
It should be noted that, in the present application, the auxiliaries are all in the prior art, and the use of the auxiliaries is not in the technical improvement of the present application, so that the present application does not describe specific components of the auxiliaries, and all the auxiliaries that can be used in the present application can be applicable.
Further preferably, the inorganic photochromic agent is CaHfO3Inorganic photochromic material as matrix material and its expression M1-X HfO3: xR and xR, wherein M is one of alkaline earth metal elements Ca, Sr and Ba; x is the doping amount of R, and x is more than or equal to 0 and less than or equal to 0.03; r is a rare earth element doped into the base material and is selected from one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
Further preferably, the organic photochromic agent includes at least one of spirobenzopyran, spiro oh, diarylethene, or azobenzene.
Another object of the present invention is to provide a method for preparing the above photochromic fiber. The preparation method has the advantages of simple process, strong operability, high production efficiency and low cost, and is suitable for popularization and application in the market.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of photochromic fibers comprises the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and polyethylene fiber or polypropylene fiber raw materials in a benign solvent, and stirring and dissolving to obtain spinning solution;
2) spinning: putting the spinning solution into a spinning system for spinning, and then carrying out solidification forming to obtain fibers;
3) and (3) washing and oiling the fiber: immersing the fiber into hot water for water washing, and then immersing the fiber into an oil bath for treatment for later use;
4) drying the fibers: and (3) drying the fiber treated in the step 3) to obtain the photochromic fiber.
Preferably, the stirring and dissolving temperature in the step 1) is 125-140 ℃, and the dissolving time is 4-6 h.
Preferably, 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; and the solidification temperature is 0-10 ℃.
Preferably, in the step 3), the washing temperature is 70-85 ℃, and the washing time is 3-5 min; the oil bath temperature is 85-95 ℃, and the treatment time is 3-5 min.
Compared with the prior art, the preparation method of the photochromic fiber disclosed by the invention has the following excellent effects:
1. the photochromic master batch and the polyethylene fiber or the polypropylene fiber have strong binding capacity, the photochromic performance of the photochromic fiber prepared by the invention is not weakened after being washed for many times, and the photochromic fiber has the advantages of wide sources of raw materials, low price, small environmental pollution in the production process and better application and popularization prospects.
2. The mechanical property of the photochromic fiber prepared by the method is superior to that of common fibers, and the photochromic agent comprises an inorganic reversible photochromic agent and an organic photochromic agent, so that the photochromic fiber has good ultraviolet photochromic property and the ultraviolet protection property of the fiber is improved;
specifically, the organic photochromic agent is used, when visible light irradiates on the fiber, the color of the fiber is lightened, the light transmittance is improved, and the color of the fiber is darkened and the light transmittance is reduced along with the reduction of the visible light, so that the heat insulation performance of the fiber is improved while the shielding performance of the fiber is ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
Example 1:
a preparation method of photochromic fibers specifically comprises the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and ultra-high molecular weight polyethylene fiber raw materials in an NMMO aqueous solution, and stirring and dissolving for 4 hours in a reaction kettle at 130 ℃ in vacuum to prepare spinning solution;
2) spinning: adding the spinning solution into a screw extruder, further dissolving at 100 ℃, then filtering, then putting the spinning solution into a spinning system for spinning, vertically stretching the sprayed silk threads in the air, then entering a coagulating bath, and coagulating and forming at 5 ℃ to obtain fibers; wherein the air gap length of the spinning system is 8cm, the spinning speed is 40m/min, the pore diameter of a spinneret plate is 60 mu m, and the length of a pore capillary is 550 mu m;
3) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at 80 ℃ for washing, wherein the washing time is 3 minutes, and the bath ratio is 1: 20;
4) oiling the fibers: immersing the fiber treated in the step 3) into 4g/L of oil bath solution, wherein the oil bath temperature is 85 ℃, the time is 4 minutes, and the bath ratio is 1: 15;
5) drying the fibers: and (3) drying the fiber treated in the step (4) to obtain the photochromic fiber.
The mass ratio of the photochromic master batch to the ultra-high molecular weight polyethylene fiber raw material is 1: 35, and the photochromic master batch is formed by mixing 70% of photochromic agent and 30% of auxiliary agent;
the auxiliary agent is one or a combination of more of an oxidant, a compatilizer, an anti-aging agent and a light stabilizer, and the auxiliary agent is not taken as the technical protection point of the invention;
the photochromic agent is made of CaHfO3：La2O3And spiropyran in a mass ratio of 1: 3, and mixing.
Example 2:
a preparation method of photochromic fibers specifically comprises the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and polypropylene fiber raw materials in DCM aqueous solution, and stirring and dissolving for 5 hours in a reaction kettle at 135 ℃ in vacuum to prepare spinning solution;
2) spinning: adding the spinning solution into a screw extruder, further dissolving at 110 ℃, then filtering, then putting the spinning solution into a spinning system for spinning, vertically stretching the sprayed silk threads in the air, then entering a coagulating bath, and coagulating and forming at 2 ℃ to obtain fibers; wherein the air gap length of the spinning system is 8cm, the spinning speed is 35m/min, the pore diameter of a spinneret plate is 80 mu m, and the length of a pore capillary is 500 mu m;
3) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at 80 ℃ for washing, wherein the washing time is 4 minutes, and the bath ratio is 1: 20;
4) oiling the fibers: immersing the fiber treated in the step 3) into 4g/L of oil bath solution, wherein the oil bath temperature is 90 ℃, the time is 4 minutes, and the bath ratio is 1: 20;
5) drying the fibers: and (3) drying the fiber treated in the step (4) to obtain the photochromic fiber.
The mass ratio of the photochromic master batch to the polypropylene fiber raw material is 1: 30, and the photochromic master batch is formed by mixing 75 percent of photochromic agent and 25 percent of auxiliary agent;
the auxiliary agent is one or a combination of more of an oxidant, a compatilizer, an anti-aging agent and a light stabilizer, and the auxiliary agent is not taken as the technical protection point of the invention;
the photochromic agent is made of CaHfO3：La2O3And azobenzene according to a mass ratio of 1: 3, and mixing.
Example 3:
a preparation method of photochromic fibers specifically comprises the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and polyethylene fiber raw materials in an NMMO aqueous solution, and dissolving in a reaction kettle at 135 ℃ for 4 hours under vacuum stirring to prepare a spinning solution;
2) spinning: adding the spinning solution into a screw extruder, further dissolving at 115 ℃, then filtering, then putting the spinning solution into a spinning system for spinning, vertically stretching the sprayed silk threads in the air, then entering a coagulating bath, and coagulating and forming at 6 ℃ to obtain fibers; wherein the air gap length of the spinning system is 8cm, the spinning speed is 40m/min, the pore diameter of a spinneret plate is 60 mu m, and the length of a pore capillary is 550 mu m;
3) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at 80 ℃ for washing, wherein the washing time is 4 minutes, and the bath ratio is 1: 25;
4) oiling the fibers: immersing the fiber treated in the step 3) into 4g/L of oil bath solution, wherein the oil bath temperature is 85 ℃, the time is 5 minutes, and the bath ratio is 1: 20;
5) drying the fibers: and (3) drying the fiber treated in the step (4) to obtain the photochromic fiber.
The mass ratio of the photochromic master batch to the polyethylene fiber raw material is 1: 40, and the photochromic master batch is formed by mixing 80 percent of photochromic agent and 20 percent of auxiliary agent;
the auxiliary agent is one or a combination of more of an oxidant, a compatilizer, an anti-aging agent and a light stabilizer, and the auxiliary agent is not taken as the technical protection point of the invention;
the photochromic agent is made of CaHfO3：La2O3And spiropyran in a mass ratio of 1: 3, and mixing.
Example 4:
a preparation method of photochromic fibers specifically comprises the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and polypropylene/polyethylene fiber raw materials in TFA aqueous solution, and dissolving in a reaction kettle at 140 ℃ under vacuum stirring for 4 hours to prepare spinning solution;
2) spinning: adding the spinning solution into a screw extruder, further dissolving at 100 ℃, then filtering, then putting the spinning solution into a spinning system for spinning, vertically stretching the sprayed silk threads in the air, then entering a coagulating bath, and coagulating and forming at 5 ℃ to obtain fibers; wherein the air gap length of the spinning system is 8cm, the spinning speed is 40m/min, the pore diameter of a spinneret plate is 60 mu m, and the length of a pore capillary is 550 mu m;
3) and (3) water washing of the fiber: soaking the fiber treated in the step 2) into hot water at 80 ℃ for washing, wherein the washing time is 3 minutes, and the bath ratio is 1: 25;
4) oiling the fibers: immersing the fiber treated in the step 3) into 4g/L of oil bath solution, wherein the oil bath temperature is 85 ℃, the time is 4 minutes, and the bath ratio is 1: 20;
5) drying the fibers: and (3) drying the fiber treated in the step (4) to obtain the photochromic fiber.
The mass ratio of the photochromic master batch to the polyethylene fiber raw material is 1: 35, and the photochromic master batch is formed by mixing 75% of photochromic agent and 25% of auxiliary agent;
the auxiliary agent is one or a combination of more of an oxidant, a compatilizer, an anti-aging agent and a light stabilizer, and the auxiliary agent is not taken as the technical protection point of the invention;
the photochromic agent is made of CaHfO3：La2O3And spiropyran in a mass ratio of 1: 3, and mixing.
In order to prove the technical effect of the invention, the performance of the photochromic fibers obtained in the embodiments 1 to 4 of the invention was tested.
The performance test comprises the following steps: and testing photochromic performance.
And (3) carrying out photochromic performance test on the photochromic fibers prepared in the specific embodiments 1-4. Wherein, the light source adopts a xenon lamp of 500W for irradiation, the irradiation time is 5 minutes, and the photochromic fibers are changed from natural color (white) to blue.
The photochromic fiber was then subjected to standard washing 20 times and the photochromic performance test was again performed, and as a result, it was found that the photochromic fiber had the same photochromic performance as before washing. The photochromic master batch and the polyethylene fiber or the polypropylene fiber have strong binding capacity, and the photochromic performance of the photochromic fiber prepared by the invention is not weakened after being washed by water for many times.
And (5) performance test II: mechanical testing of fibers
The photochromic fibers prepared in the specific embodiments 1 to 4 are subjected to mechanical property tests, and the test method refers to GB/T-24218.3-2010 test method for textiles 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:
TABLE 1 fiber mechanical Properties data
As can be seen from Table 1, the dry breaking strength of the photochromic fibers is between 55 and 70cN/tex, which is higher than that of the commercially available fibers, and the dry breaking elongation of the photochromic fibers is between 18 and 20 percent, which is higher than that of the commercially available fibers; the wet breaking strength of the photochromic fiber is 42-55 cN/tex which is higher than that of the commercially available fiber, and the wet breaking elongation of the photochromic fiber is 16-17% which is higher than that of the commercially available fiber, so that the mechanical property of the photochromic fiber is better than that of the commercially available fiber from the test result of the mechanical property. Therefore, the photochromic fiber prepared by the method is a qualified fiber, and the preparation method is simple and efficient, is suitable for large-scale production, and has good market application prospect.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The photochromic fiber is characterized in that the fiber is prepared by mixing photochromic master batch into a spinning solution of polyethylene fiber or polypropylene fiber raw material for spinning; wherein the content of the first and second substances,
the mass ratio of the photochromic master batch to the polyethylene fiber or polypropylene fiber raw material is 1: (30-40), wherein the photochromic master batch is formed by mixing a photochromic agent and an auxiliary agent;
the photochromic agent is prepared from an inorganic photochromic agent and an organic photochromic agent according to a mass ratio of 1: 3, and mixing.
2. The photochromic fiber of claim 1, wherein the benign solvent of the spinning solution is NMMO, TFA or DCM, and the mass concentration of the spinning solution is 10-15%.
3. The photochromic fiber of claim 1, wherein the photochromic master batch is prepared by mixing a photochromic agent and an auxiliary agent, and the photochromic agent comprises the following components in percentage by mass:
65-85% of photochromic agent,
15-30% of an auxiliary agent.
4. The photochromic fiber of claim 3 wherein the auxiliary agent comprises one or more of an oxidant, a compatibilizer, an anti-aging agent, and a light stabilizer.
5. The photochromic fiber of claim 1 or 3 wherein the inorganic photochromic agent is CaHfO3Inorganic photochromic material as matrix material and its expression M1-XHfO3: xR and xR, wherein M is one of alkaline earth metal elements Ca, Sr and Ba; x is the doping amount of R, and x is more than or equal to 0 and less than or equal to 0.03; r is a rare earth element doped into the base material and is selected from one or more of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
6. The photochromic fiber of claim 1 or 3 wherein the organic photochromic agent comprises at least one of spiropyran, spiro oh, diarylethene, or azobenzene.
7. A method for preparing the photochromic fiber according to any one of claims 1 to 6, comprising the following steps:
1) preparing a spinning solution: dissolving photochromic master batch and polyethylene fiber or polypropylene fiber raw materials in a benign solvent, and stirring and dissolving to obtain spinning solution;
2) spinning: putting the spinning solution into a spinning system for spinning, and then carrying out solidification forming to obtain fibers;
3) and (3) washing and oiling the fiber: immersing the fiber into hot water for water washing, and then immersing the fiber into an oil bath for treatment for later use;
4) drying the fibers: and (3) drying the fiber treated in the step 3) to obtain the photochromic fiber.
8. The preparation method of the photochromic fiber according to claim 7, wherein the stirring and dissolving temperature in the step 1) is 125-140 ℃, and the dissolving time is 4-6 h.
9. The method for preparing the photochromic fiber according to claim 7, wherein in the step 2), the air gap length of a spinning system is 7-9 cm, the spinning speed is 35-55 m/min, the pore diameter of a spinneret plate is 15-115 μm, and the length of a pore capillary is 350-800 μm; and the solidification temperature is 0-10 ℃.
10. The preparation method of the photochromic fiber according to claim 7, wherein in the step 3), the washing temperature is 70-85 ℃ and the washing time is 3-5 min; the oil bath temperature is 85-95 ℃, and the treatment time is 3-5 min.
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Cited By (1)
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| 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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