CN115491792A - Photo-curing spinning oil and preparation method and application thereof - Google Patents

Photo-curing spinning oil and preparation method and application thereof Download PDF

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CN115491792A
CN115491792A CN202211382600.XA CN202211382600A CN115491792A CN 115491792 A CN115491792 A CN 115491792A CN 202211382600 A CN202211382600 A CN 202211382600A CN 115491792 A CN115491792 A CN 115491792A
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parts
long
photocuring
luminescent material
spinning oil
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CN115491792B (en
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王山水
王丽丽
汤方明
魏存宏
王雪
张元华
张怡
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Jiangsu Hengli Chemical Fiber Co Ltd
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Jiangsu Hengli Chemical Fiber Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/08Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Artificial Filaments (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention relates to a photo-curing spinning oil agent and a preparation method and application thereof, wherein the spinning oil agent comprises the following components in parts by weight: the material comprises, by weight, 5 to 10 parts of a long-afterglow luminescent material containing double bonds, 40 to 60 parts of vinyl silicone oil and 2 to 5 parts of a photoinitiator, wherein the photoinitiator is a substance capable of initiating a crosslinking reaction between the long-afterglow luminescent material containing double bonds and the vinyl silicone oil under the illumination condition; the preparation method comprises the following steps: mixing the components according to the proportion, and uniformly stirring at 25 to 35 ℃ to obtain a photocuring spinning oil; the application comprises the following steps: oiling adopts the spinning oil agent; the next procedure of the stretching procedure is a photocuring procedure; the product solves the problems of poor compatibility between the luminous filler and the oil agent, easy migration and precipitation, uneven luminescence and difficult persistence of the existing compound fluorescent oil agent; the method of the invention is simple to prepare; the invention is applied to the fiber, shows excellent cycle energy storage-luminescence characteristics, and has no solvent discharge and cleanness.

Description

Photo-curing spinning oil and preparation method and application thereof
Technical Field
The invention belongs to the technical field of spinning oil agents, and relates to a photo-curing spinning oil agent and a preparation method and application thereof.
Background
The spinning oil is an assistant for reducing the static electricity and friction coefficient between fibers in the spinning process and further ensuring good spinnability and post-processing property. With the continuous development of society, single-performance industrial yarn products cannot meet the social demands, and industrial yarn products with functions of luminescence, color change, flame retardance, antibiosis and the like are favored by consumers.
The long-afterglow luminescent material can store external light irradiation energy, absorb light for storage when the light is sufficient, and release the light in the form of visible light under the dark condition, so the long-afterglow luminescent material is also called as an energy storage luminescent material. The rare earth metal excited alkaline earth aluminate series luminescent material has the advantages of high luminescent efficiency, long afterglow time, stable chemical property, no radioactive hazard and the like, and is always valued by people. The long-afterglow luminescent material is combined with the industrial yarn, so that the long-afterglow luminescent material can be endowed with new luminescent characteristics, can be used for work articles for night work, such as automobiles, deep well/high altitude work hauling ropes, ropes for climbers and the like, provides convenient conditions for the work of night workers, and has a self-luminescent function so as to facilitate the tracking and timely carry out rescue work when danger occurs.
CN111394822A discloses a fluorescent fiber and a manufacturing method thereof, wherein the fluorescent fiber is manufactured by a melt spinning process: firstly, mixing a fluorescent substance and a spinning oil agent to prepare an oil agent mixed solution, coating the oil agent mixed solution on the surface of a fiber in a spinning oiling mode when a polymer melt is extruded by a spinneret plate and stretched into the fiber in a melt spinning process, and then coiling and forming to obtain the fluorescent fiber, wherein the total fineness of the fluorescent fiber is 900-3300 dtex, the fiber strength is not less than 7.0cN/dtex, the oil content of the fiber is 0.3-0.9%, and the fiber is polyethylene terephthalate, nylon 66 or nylon 6.
On one hand, however, most fluorescent materials are inorganic materials, and physical compounding of the fluorescent materials and the oil solution can easily cause the delamination or precipitation of the spinning oil solution under the condition of no modification; on the other hand, the simple physical blending can also cause that the luminescent micromolecules are easy to migrate and fall off in the using process of the industrial yarn, the luminescent performance is difficult to maintain for a long time, and further the product quality is influenced.
Therefore, the research on the photo-curing spinning oil agent and the preparation method and the application thereof to solve the problems has very important significance.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a photo-curing spinning oil agent and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a light-curing spinning oil comprises, by weight, 5 to 10 parts of a long-afterglow luminescent material containing double bonds, 40 to 60 parts of vinyl silicone oil and 2 to 5 parts of a photoinitiator, wherein the photoinitiator is a substance capable of initiating a crosslinking reaction between the long-afterglow luminescent material containing the double bonds and the vinyl silicone oil under the illumination condition.
The long afterglow luminescent material determines the energy storage luminescent performance, is a filler, and can cause the flexibility of the coating to be reduced after the oil agent is cured and the comprehensive physical performance to be reduced when the long afterglow luminescent material is too large; if the content is too small, the luminous performance at night cannot meet the requirement; 5 to 10 portions are the range of the comprehensive optimized dosage interval; vinyl silicone oil is a main film forming substance, and is matched with a luminescent material and a photoinitiator according to the proportion, so that the comprehensive performance can be optimal; the using amount of the photoinitiator determines the photocuring time, the time is shortened when the photoinitiator is too large, the time is prolonged when the photoinitiator is too small, and 2 to 5 parts are the preferable using amount according to the curing time of 2 to 4s.
As a preferred technical scheme:
the preparation process of the long afterglow luminescent material containing double bonds comprises the following steps: 10 to 20 parts by weight of long afterglow luminescent material SrAl 2 O 4 : Eu 2+ , Dy 3+ Mixing with 6 to 8 parts of silane coupling agent gamma-methacryloxypropyltrimethoxysilane, vinyl trimethoxysilane or vinyl triethoxysilane, adjusting the pH value of the system to be 3 to 4, reacting at 50 to 60 ℃ for 3 to 5 hours, and performing post-treatment (ammonia water)Neutralizing, washing with ethanol, purifying and drying) to obtain the long-afterglow luminescent material containing double bonds.
The photo-curable spinning oil is vinyl silicone oil with double bonds at both end groups and side chains, wherein the content of vinyl is 10 to 12wt%.
The photo-curing spinning oil is characterized in that the photoinitiator is more than one of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl acetone and isopropyl thioxanthone.
The photocurable spinning oil further comprises, by weight, 15 to 25 parts of an antistatic agent, 10 to 20 parts of an active diluent and 3 to 5 parts of a surfactant. The reactive diluent reduces the viscosity of the system on one hand, and ensures the operability of the oiling process; on the other hand, the diluent contains 3 to 4 double bonds of active functional groups, and a compact cross-linking structure of the finally cured coating can be endowed through photocuring, so that the stability of the coating is ensured.
The photo-curing spinning oil is characterized in that the antistatic agent is long-alkyl dimethyl hydroxyethyl quaternary ammonium salt and/or fatty alcohol polyoxyethylene potassium phosphate;
the active diluent is more than one of ethoxylated trimethylolpropane triacrylate, propoxylated trimethylolpropane triacrylate and ethoxylated pentaerythritol tetraacrylate;
the surfactant is more than one of fatty alcohol polyoxyethylene ether AEO-5, AEO-7 or AEO-9.
The invention also provides a method for preparing the photocuring spinning oil, which comprises the steps of mixing the components according to the proportion, and uniformly stirring at 25-35 ℃ to obtain the photocuring spinning oil.
The invention also provides a preparation method of the energy storage luminous polyester industrial yarn, which comprises an oiling process and a stretching process, wherein the oiling agent is the photo-curing spinning oil agent; the subsequent step of the stretching step is a photocuring step, and the photocuring step is a step of initiating the crosslinking reaction between the long-afterglow luminescent material containing double bonds and the vinyl silicone oil by using a photocuring spinning oil agent which irradiates the surface of the fiber with light.
As a preferable technical scheme:
according to the preparation method of the energy storage luminous polyester industrial yarn, the light source for photocuring is 5 mercury lamps of 1387 mm mercury in British Primarc 9.7 KW, and the photocuring time is 2 to 4s.
The preparation method of the energy-storage luminous polyester industrial yarn comprises the following specific process flows: melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming.
According to the preparation method of the energy storage luminous polyester industrial yarn, the energy storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 abrasion resistance of fabrics by Martindale method, and after being rubbed 3000 times, the cloth still has energy storage-luminous characteristics.
Advantageous effects
(1) The silane coupling agent containing double bonds is used for modifying the long-afterglow luminescent material and is introduced into a photocuring system of a reaction type oil agent in a covalent form, so that the problems of poor compatibility, easy migration and precipitation, uneven distribution, poor luminescent property durability, poor stability and the like of the conventional blending compound luminescent material and a spinning oil agent are solved;
(2) The energy-storage luminous polyester industrial yarn prepared by the invention can absorb sunlight for storage in the daytime and release in a visible light mode at night, so that the functionality of the industrial yarn can be increased, the luminous cycle times can be increased, and the application field of the industrial yarn can be greatly widened;
(3) By adopting the photocuring crosslinking technology, the chemical problem is solved by a physical method, the energy consumption is lower, the efficiency is higher, the used raw materials do not contain any organic solvent, compared with the traditional solvent type spinning oil, the pollution of the organic solvent is eliminated from the source, the product does not contain VOCs, and the product quality and the ecological grade can be effectively improved.
Detailed Description
The present invention will be further described with reference to the following embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
The method for testing the energy storage-luminescence characteristics in the following examples is as follows:
the afterglow decay time is measured by an afterglow characteristic testing system of a CY-1000B light-storing material of remote spectral color technology limited, and a sample is pre-excited for 5 minutes under a light source with the color temperature of 4500K and the illumination of 1000lx before the afterglow decay measurement.
Example 1
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: gamma-methacryloxypropyltrimethoxysilane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): 1-hydroxycyclohexyl phenyl ketone;
antistatic agent: octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate;
active diluent: ethoxylated trimethylolpropane triacrylate;
surfactant (b): AEO-5;
(2) Preparing a spinning oil agent:
(2.1) mixing 10 parts of long-afterglow luminescent material and 6 parts of silane coupling agent in parts by weight, adjusting the pH value of the system to 3 after mixing, reacting for 3 hours at 50 ℃, then drying the product after ammonia neutralization, ethanol washing and purification to prepare the long-afterglow luminescent material containing double bonds;
(2.2) mixing 10 parts by weight of double-bond-containing long-afterglow luminescent material, 40 parts by weight of vinyl silicone oil, 5 parts by weight of photoinitiator, 15 parts by weight of antistatic agent, 20 parts by weight of reactive diluent and 5 parts by weight of surfactant, and uniformly stirring at 25 ℃ to obtain the photocuring spinning oil.
The energy storage luminous polyester industrial yarn is prepared by adopting the prepared light-cured spinning oil agent, and the process flow is as follows:
melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process is to irradiate the photocuring spinning oil on the surface of the fiber for 2s by using a 5-British Primarc 9.7 KW 1387 mm mercury lamp to initiate the crosslinking reaction of the long-afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 12 hours, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 textile Martindale method fabric wear resistance, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 11.5 hours.
Comparative example 1
The preparation method of the energy-storage luminous polyester industrial yarn is basically the same as that of the embodiment 1, and is different only in a lightless curing process.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 12 hours, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 textile Martindale method fabric wear resistance, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 0.5 hour.
Comparing example 1 with comparative example 1, it can be seen that the luminescent performance durability and stability of the energy storage luminescent polyester industrial yarn of comparative example 1 are significantly lower than those of example 1, because comparative example 1 is not subjected to photocuring treatment, the long afterglow luminescent material containing double bonds cannot generate crosslinking reaction with vinyl silicone oil, and is only mixed with vinyl silicone oil, and the long afterglow luminescent material containing double bonds is easy to fall off from the fiber during use.
Example 2
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: gamma-methacryloxypropyltrimethoxysilane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): 2-hydroxy-2-methyl-1-phenylpropanone;
antistatic agent: octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate;
active diluent: propoxylated trimethylolpropane triacrylate;
surfactant (B): AEO-7;
(2) Preparing a spinning oil agent:
(2.1) mixing 15 parts by weight of long-afterglow luminescent material and 7 parts by weight of silane coupling agent, adjusting the pH value of the system to 4 after mixing, reacting for 4 hours at 60 ℃, drying the product after ammonia neutralization, ethanol washing and purification, and obtaining the long-afterglow luminescent material containing double bonds;
(2.2) mixing 8 parts by weight of double-bond-containing long-afterglow luminescent material, 50 parts by weight of vinyl silicone oil, 2 parts by weight of photoinitiator, 25 parts by weight of antistatic agent, 10 parts by weight of active diluent and 4 parts by weight of surfactant, and uniformly stirring at 30 ℃ to obtain the photocuring spinning oil.
The energy storage luminous polyester industrial yarn is prepared by adopting the prepared light-cured spinning oil agent, and the process flow is as follows:
melting a polyester raw material → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process is to irradiate 5 British Primarc 9.7 KW 1387 mm mercury lamps on the surface of the fiber for 4s to initiate the crosslinking reaction between the long-afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 10 hours, a friction test is carried out on the cloth according to GB/T21196.1-4-2007 abrasion resistance of fabrics by Martindale method, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 9.8 hours.
Example 3
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: gamma-methacryloxypropyltrimethoxysilane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): isopropyl thioxanthone;
antistatic agent: potassium fatty alcohol polyoxyethylene phosphate;
active diluent: ethoxylated pentaerythritol tetraacrylate;
surfactant (b): AEO-9;
(2) Preparing a spinning oil agent:
(2.1) mixing 20 parts by weight of long-afterglow luminescent material and 8 parts by weight of silane coupling agent, adjusting the pH value of the system to 4 after mixing, reacting for 5 hours at 60 ℃, then drying the product after ammonia neutralization, ethanol washing and purification to prepare the long-afterglow luminescent material containing double bonds;
(2.2) mixing 5 parts by weight of double-bond-containing long-afterglow luminescent material, 60 parts by weight of vinyl silicone oil, 5 parts by weight of photoinitiator, 20 parts by weight of antistatic agent, 20 parts by weight of reactive diluent and 3 parts by weight of surfactant, and uniformly stirring at 35 ℃ to obtain the photocuring spinning oil.
The energy storage luminous polyester industrial yarn is prepared by adopting the prepared light-cured spinning oil agent, and the process flow is as follows:
melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process is to irradiate the photocuring spinning oil on the surface of the fiber for 2s by using a 5-British Primarc 9.7 KW 1387 mm mercury lamp to initiate the crosslinking reaction of the long-afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 7 hours, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 textile Martindale method fabric wear resistance, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 6.8 hours.
Example 4
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: vinyl trimethoxy silane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): 1-hydroxycyclohexyl phenyl ketone;
antistatic agent: octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate;
active diluent: ethoxylated trimethylolpropane triacrylate;
surfactant (b): a mixture of AEO-7 and AEO-9 in a mass ratio of 50;
(2) Preparing a spinning oil agent:
(2.1) mixing 13 parts by weight of long-afterglow luminescent material and 6 parts by weight of silane coupling agent, adjusting the pH value of the system to 3 after mixing, reacting for 3.5 hours at 53 ℃, drying the product after ammonia neutralization, ethanol washing and purification, and obtaining the long-afterglow luminescent material containing double bonds;
(2.2) mixing 9 parts by weight of double-bond-containing long-afterglow luminescent material, 45 parts by weight of vinyl silicone oil, 2 parts by weight of photoinitiator, 17 parts by weight of antistatic agent, 13 parts by weight of reactive diluent and 5 parts by weight of surfactant, and uniformly stirring at 25 ℃ to obtain the light-curing spinning oil.
The energy-storage luminous polyester industrial yarn is prepared by adopting the prepared photo-curing spinning oil agent, and the process flow is as follows:
melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process is to irradiate 5 British Primarc 9.7 KW 1387 mm mercury lamps on the surface of the fiber for 4s to initiate the crosslinking reaction between the long-afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 11 hours, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 textile Martindale method fabric wear resistance, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 10.6 hours.
Example 5
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: vinyltriethoxysilane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): isopropyl thioxanthone;
antistatic agent: potassium fatty alcohol polyoxyethylene phosphate;
active diluent: a mixture of propoxylated trimethylolpropane triacrylate and ethoxylated pentaerythritol tetraacrylate in a mass ratio of 50;
surfactant (b): AEO-7;
(2) Preparing a spinning oil agent:
(2.1) mixing 15 parts by weight of long-afterglow luminescent material and 7 parts by weight of silane coupling agent, adjusting the pH value of the system to 3.5 after mixing, reacting for 4.5 hours at 55 ℃, drying the product after ammonia neutralization, ethanol washing and purification, and obtaining the long-afterglow luminescent material containing double bonds;
(2.2) mixing 7 parts by weight of long-afterglow luminescent material containing double bonds, 50 parts by weight of vinyl silicone oil, 3 parts by weight of photoinitiator, 19 parts by weight of antistatic agent, 15 parts by weight of active diluent and 4 parts by weight of surfactant, and uniformly stirring at 30 ℃ to obtain the photocuring spinning oil.
The energy storage luminous polyester industrial yarn is prepared by adopting the prepared light-cured spinning oil agent, and the process flow is as follows:
melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process adopts 5 British Primarc 9.7 KW 1387 mm mercury lamps to irradiate the photocuring spinning oil solution on the surface of the fiber for 4s to initiate the crosslinking reaction of the long afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 9 hours, a friction test is carried out on the cloth according to GB/T21196.1-4-2007 abrasion resistance of fabrics by Martindale method, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 8.8 hours.
Example 6
A preparation method of a photo-curing spinning oil agent comprises the following specific steps:
(1) Preparing raw materials:
long afterglow luminescent materials: srAl 2 O 4 : Eu 2+ , Dy 3+
Silane coupling agent: vinyltriethoxysilane;
vinyl silicone oil: the manufacturer is Zhejiang thoroughfare orange organosilicon company, and the mark is VM-26;
photoinitiator (2): a mixture of 1-hydroxycyclohexyl phenyl ketone and 2-hydroxy-2-methyl-1-phenyl acetone in a mass ratio of 50;
antistatic agent: the mass ratio of the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate to the fatty alcohol polyoxyethylene potassium phosphate is 50;
active diluent: propoxylated trimethylolpropane triacrylate;
surfactant (b): AEO-5;
(2) Preparing a spinning oil agent:
(2.1) mixing 17 parts by weight of long-afterglow luminescent material and 8 parts by weight of silane coupling agent, adjusting the pH value of the system to 4 after mixing, reacting for 5 hours at 57 ℃, then neutralizing by ammonia water, washing by ethanol, purifying, and drying the product to prepare the long-afterglow luminescent material containing double bonds;
(2.2) mixing 6 parts by weight of double-bond-containing long-afterglow luminescent material, 55 parts by weight of vinyl silicone oil, 4 parts by weight of photoinitiator, 23 parts by weight of antistatic agent, 17 parts by weight of active diluent and 3 parts by weight of surfactant, and uniformly stirring at 35 ℃ to obtain the photocuring spinning oil.
The energy-storage luminous polyester industrial yarn is prepared by adopting the prepared photo-curing spinning oil agent, and the process flow is as follows:
melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming;
wherein, the photocuring process is to irradiate 5 British Primarc 9.7 KW 1387 mm mercury lamps on the surface of the fiber with photocuring spinning oil for 3s to initiate the crosslinking reaction between the long-afterglow luminescent material containing double bonds and vinyl silicone oil.
The prepared energy-storage luminous polyester industrial yarn is woven according to a plain weave mode to obtain cloth, an afterglow characteristic testing system is used for testing, the luminous time is 8 hours, the cloth is subjected to a friction test according to GB/T21196.1-4-2007 textile Martindale method fabric wear resistance, after the cloth is rubbed 3000 times, the afterglow characteristic testing system is used for testing, and the luminous time is 7.6 hours.

Claims (10)

1. A photo-curing spinning oil agent is characterized by comprising, by weight, 5 to 10 parts of a long-afterglow luminescent material containing double bonds, 40 to 60 parts of vinyl silicone oil and 2 to 5 parts of a photoinitiator, wherein the photoinitiator is a substance capable of initiating a crosslinking reaction between the long-afterglow luminescent material containing double bonds and the vinyl silicone oil under the illumination condition.
2. The photo-curing spinning oil as claimed in claim 1, wherein the preparation process of the long afterglow luminescent material containing double bonds comprises: 10 to 20 portions of long afterglow luminescent material SrAl 2 O 4 : Eu 2+ , Dy 3+ And 6 to 8 parts of silane coupling agent gamma-methacryloxypropyltrimethoxysilane, vinyl trimethoxysilane or vinyl triethoxysilane are mixed, the pH value of the system is adjusted to be 3 to 4, and the mixture reacts for 3 to 5 hours at the temperature of 50 to 60 ℃ for post-treatment, so that the long-afterglow luminescent material containing double bonds is obtained.
3. The photocurable spin finish of claim 1, wherein the vinyl silicone oil is a vinyl silicone oil containing double bonds in both the terminal group and the side chain, and the vinyl content is 10 to 12wt%.
4. The photocurable spin finish according to claim 1, wherein the photoinitiator is at least one of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl acetone, and isopropyl thioxanthone.
5. The photo-curable spinning oil as claimed in claim 1, further comprising 15 to 25 parts by weight of an antistatic agent, 10 to 20 parts by weight of an active diluent, and 3 to 5 parts by weight of a surfactant.
6. The photo-curable spinning oil as defined in claim 5, wherein the antistatic agent is long-alkyl dimethyl hydroxyethyl quaternary ammonium salt and/or fatty alcohol polyoxyethylene phosphate potassium salt;
the active diluent is more than one of ethoxylated trimethylolpropane triacrylate, propoxylated trimethylolpropane triacrylate and ethoxylated pentaerythritol tetraacrylate;
the surfactant is one or more of fatty alcohol-polyoxyethylene ether AEO-5, AEO-7 or AEO-9.
7. The method for preparing the photocuring spinning oil as defined in any one of claims 1 to 6, wherein the photocuring spinning oil is obtained by mixing the components according to the proportion and then uniformly stirring at 25 to 35 ℃.
8. A preparation method of an energy storage luminous polyester industrial yarn comprises an oiling process and a stretching process, and is characterized in that an oil agent used for oiling is a light-curing spinning oil agent according to any one of claims 1 to 6; the subsequent step of the stretching step is a photocuring step, and the photocuring step is a step of initiating the crosslinking reaction between the long-afterglow luminescent material containing double bonds and the vinyl silicone oil by using a photocuring spinning oil agent which irradiates the surface of the fiber with light.
9. The method for preparing the energy storage luminous polyester industrial yarn as claimed in claim 8, wherein the photocuring time is 2 to 4s.
10. The preparation method of the energy storage luminous polyester industrial yarn according to claim 8, characterized in that the specific process flow is as follows: melting polyester raw materials → metering → spinning → cooling → oiling → stretching → photocuring → winding and forming.
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