CN116552063B - Fabric with night light reflecting effect and preparation process - Google Patents

Fabric with night light reflecting effect and preparation process Download PDF

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Publication number
CN116552063B
CN116552063B CN202310841684.7A CN202310841684A CN116552063B CN 116552063 B CN116552063 B CN 116552063B CN 202310841684 A CN202310841684 A CN 202310841684A CN 116552063 B CN116552063 B CN 116552063B
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Prior art keywords
fabric
layer
light reflecting
polyurethane adhesive
isophorone diisocyanate
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CN116552063A (en
Inventor
谢秉政
杨思思
代丽娟
唐新乔
张明星
陈佳
裴登峰
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Guangdong BiemLFdlkk Golf Garment Co ltd
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Guangdong BiemLFdlkk Golf Garment Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/44—Polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6655—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/12—Reflex reflectors
    • G02B5/126—Reflex reflectors including curved refracting surface
    • G02B5/128—Reflex reflectors including curved refracting surface transparent spheres being embedded in matrix
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0276—Polyester fibres
    • B32B2262/0284—Polyethylene terephthalate [PET] or polybutylene terephthalate [PBT]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/06—Vegetal fibres
    • B32B2262/062—Cellulose fibres, e.g. cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/14—Mixture of at least two fibres made of different materials

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Fluid Mechanics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention relates to the field of fabric preparation, in particular to a fabric with a night light reflecting effect and a preparation process, wherein the fabric comprises a basic fabric layer, a light reflecting material layer and a bonding layer, wherein the bonding layer is arranged between the basic fabric layer and the light reflecting material layer, the bonding layer is a modified polyurethane adhesive, and the modified polyurethane adhesive is synthesized by using isophorone diisocyanate and polycarbonate diol as reactants under the action of a modified chain extender. The invention improves the bonding layer between the base layer and the reflective layer of the fabric, so that the bonding part between the reflective layer and the fabric base layer is not easy to yellow or fall off after the fabric is worn for a long time or washed.

Description

Fabric with night light reflecting effect and preparation process
Technical Field
The invention relates to the field of fabric preparation, in particular to a fabric with a night light reflecting effect and a preparation process thereof.
Background
Retroreflective garments are garments having a high degree of retroreflective properties and are typically made from retroreflective materials. The material can reflect light rays, so that people can be more easily noticed by other people or vehicles in dark places or in low-visibility environments, and the safety is improved. Retroreflective garments are commonly used for night walking, riding, working, or other applications where low visibility environments are desired, such as police, traffic police, construction workers, and other professionals often wear retroreflective garments to improve their visibility and safety on traffic roads.
The reflective clothing is made of reflective materials, which can reflect light and improve the visibility and safety of people in low-visibility environments. Retroreflective materials generally include the following: 1. high visibility retroreflective material: the material is made of high-reflectivity polymer, has very high reflectivity, and is generally used in clothing for professionals such as police, firefighters, road construction personnel and the like. 2. Glass bead reflecting material: the material is made of glass beads, and is suitable for outdoor exercises, running at night and other occasions. 3. Reflective cloth: such materials are made of polyester fibers and are commonly used to make reflective vests, reflective garments, and the like. 4. Reflective sticker: the material is usually attached to the surface of articles such as clothing, backpacks and the like, and can reflect light under the irradiation of light so as to improve the visibility of people.
Along with the improvement of living standard, the comfort and the function of the clothing articles are also increasingly required. The reflective clothing is usually formed by bonding a layer of reflective material on the surface of the fabric, so that the reflective material reflects intense light under the irradiation of light, and the visibility and the safety of a wearer are improved. However, the adhesion of the reflective layer of the reflective fabric on the market is poor, the reflective fabric is easy to fall off, and the reflective fabric is easy to yellow in the long-term use process, so that the appearance and the warning effect of the fabric are greatly affected.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a fabric with a night light reflecting effect and a preparation process thereof.
The aim of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides a fabric with a night light reflecting effect, which comprises a basic fabric layer, a light reflecting material layer and a bonding layer, wherein the bonding layer is arranged between the basic fabric layer and the light reflecting material layer, the bonding layer is a modified polyurethane adhesive, and the modified polyurethane adhesive is synthesized by using isophorone diisocyanate and polycarbonate diol as reactants under the action of a modified chain extender.
Preferably, the component of the basic fabric layer is any one of polyester, cotton, hemp, polyester-cotton blending, polyester-hemp blending and cotton-hemp blending.
Preferably, the reflective material layer is a cloth bonded with glass beads or a cloth coated with phosphorescent paint, and the material of the cloth is generally polyester fabric.
Preferably, the light reflecting material layer is fixed with the base fabric layer in a partially covered manner, wherein the partially covered refers to that the coverage area of the light reflecting material layer on the surface of the base fabric layer is less than 50%.
Preferably, the preparation method of the modified polyurethane adhesive comprises the following steps:
s1, under the condition of room temperature, weighing N, N-dimethylformamide, placing the N, N-dimethylformamide into a three-neck flask, adding sodium hydroxide to adjust the pH to 11.0-12.0, uniformly stirring, adding ethylene glycol diglycidyl ether and 2-amino-4-hydroxy-6-methylpyrimidine, and uniformly stirring at room temperature to form an intermediate reaction solution;
s2, gradually heating the intermediate reaction liquid to 50-60 ℃, stirring the reaction liquid at a speed of 300-500r/min, carrying out heat preservation reaction for 3-10h, naturally cooling to room temperature, and removing the solvent to obtain the modified chain extender;
s3, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 70-80 ℃, introducing nitrogen as a shielding gas, sequentially adding isophorone diisocyanate and a catalyst, and carrying out heat preservation reaction for 2-3 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
s4, adding a modified chain extender into the prepolymerization reaction mixture, continuing to perform heat preservation reaction for 1-3h, then cooling to 40-50 ℃, adding triethylamine, performing heat preservation stirring for 10-20min, and adding ethyl acetate to adjust the solid content after the reaction is finished, thus obtaining the modified polyurethane adhesive.
Preferably, in the S1, the mass ratio of the ethylene glycol diglycidyl ether, the 2-amino-4-hydroxy-6-methyl pyrimidine and the N, N-dimethylformamide is 1.7-3.4:1.2-2.4:10-20.
Preferably, in the step S3, the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1-1.2:1.
Preferably, in the step S3, the catalyst is dibutyl tin dilaurate, and the addition amount is 0.2% -0.6% of the mass of isophorone diisocyanate.
Preferably, in the step S4, the mass ratio of the addition amount of the modified chain extender to the isophorone diisocyanate in the step S3 is 1:5-10.
Preferably, in the step S4, the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in the step S3 is 1:8-16.
Preferably, in the step S4, the solid content of the modified polyurethane adhesive is 55% -85%.
In a second aspect, the invention provides a process for preparing a fabric with a night light reflecting effect, which comprises the following steps:
coating a modified polyurethane adhesive on the non-reflective surface of the reflective material layer, then bonding the surface to the part of the basic fabric layer to be bonded, heating to 55-60 ℃, carrying out hot pressing treatment for 1-3min, and cooling to obtain the fabric with the night reflective effect.
Preferably, the sizing amount of the modified polyurethane adhesive on the reflecting material layer is 15-35g/m 2 。
The beneficial effects of the invention are as follows:
1. the fabric with the night light-reflecting effect is prepared by the method, and the problems that the existing light-reflecting fabric is insufficient in adhesive effect, easy to yellow in the use period and easy to fall off in the light-reflecting layer are mainly solved. The invention improves the bonding layer between the base layer and the reflective layer of the fabric, so that the bonding part between the reflective layer and the fabric base layer is not easy to yellow or fall off after the fabric is worn for a long time or washed.
2. The invention improves the adhesive layer of the fabric layer, wherein the adhesive layer uses a modified polyurethane adhesive, the modified polyurethane adhesive uses isophorone diisocyanate and polycarbonate diol as reactants, and a modified chain extender is added for chain extension treatment, so that the obtained modified polyurethane has stronger adhesive effect and stronger washing resistance and ageing resistance.
3. The preparation process of the modified polyurethane adhesive comprises the following steps: mixing ethylene glycol diglycidyl ether containing double-end epoxy groups and 2-amino-4-hydroxy-6-methyl pyrimidine containing amino groups, hydroxy groups and pyrimidine groups under alkaline conditions, and then reacting the ethylene glycol diglycidyl ether with the 2-amino-4-hydroxy-6-methyl pyrimidine to obtain a compound containing polyhydroxy groups by utilizing the ring-opening combination characteristic of the amino groups and the epoxy groups under the condition of heating; the polyhydroxy compound is used as a chain extender, so that the molecular weight of a prepolymer product of isophorone diisocyanate and polycarbonate diol is further extended, and a pyrimidine group and an epoxy group after ring opening are simultaneously introduced into a polyurethane compound, so that the modified polyurethane adhesive is finally obtained.
Detailed Description
The technical scheme of the invention is described below through specific examples. It is to be understood that the mention of one or more method steps of the present invention does not exclude the presence of other method steps before and after the combination step or that other method steps may be interposed between these explicitly mentioned steps; it should also be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the method steps is merely a convenient tool for identifying the method steps and is not intended to limit the order of arrangement of the method steps or to limit the scope of the invention in which the invention may be practiced, as such changes or modifications in their relative relationships may be regarded as within the scope of the invention without substantial modification to the technical matter.
In order to better understand the above technical solution, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention are shown, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The invention is further described with reference to the following examples.
Example 1
The utility model provides a surface fabric with effect of reflection of light night, includes basic surface course, reflection of light material layer and tie coat, and wherein, the tie coat sets up between basic surface course and reflection of light material layer, and the tie coat is modified polyurethane adhesive, and the composition of basic surface course is the dacron, reflection of light material layer is the dacron cloth that bonds there is glass bead.
The light reflecting material layer is fixed with the base fabric layer in a partial coverage mode, wherein the partial coverage means that the coverage area of the light reflecting material layer on the surface of the base fabric layer is less than 50%.
The preparation method of the modified polyurethane adhesive comprises the following steps:
s1, under the condition of room temperature, weighing N, N-dimethylformamide, placing the N, N-dimethylformamide into a three-neck flask, adding sodium hydroxide to adjust the pH to 11.0-12.0, uniformly stirring, adding ethylene glycol diglycidyl ether and 2-amino-4-hydroxy-6-methylpyrimidine, and uniformly stirring at room temperature to form an intermediate reaction solution;
wherein the mass ratio of the ethylene glycol diglycidyl ether to the 2-amino-4-hydroxy-6-methylpyrimidine to the N, N-dimethylformamide is 2.6:1.8:15.
S2, gradually heating the intermediate reaction liquid to 50 ℃, stirring the reaction liquid at the speed of 400r/min, carrying out heat preservation reaction for 6 hours, naturally cooling to room temperature, and removing the solvent to obtain the modified chain extender;
s3, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 75 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 2 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1.1:1; the addition amount of dibutyl tin dilaurate is 0.4% of the mass of isophorone diisocyanate.
S4, adding a modified chain extender into the prepolymerization reaction mixture, continuing to perform heat preservation reaction for 2 hours, then cooling to 45 ℃, adding triethylamine, performing heat preservation stirring for 15 minutes, and adding ethyl acetate to adjust the solid content to 75% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the modified chain extender to the isophorone diisocyanate in S3 is 1:8, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in S3 is 1:12.
The preparation process of the fabric with the night light reflecting effect comprises the following steps:
coating the non-reflective surface of the reflective material layer with modified polyurethane adhesive with the sizing amount of 25g/m 2 And then bonding the base fabric layer at the position to be bonded, heating to 60 ℃, carrying out hot pressing treatment for 2min, and cooling to obtain the fabric with the night light reflection effect.
Example 2
The utility model provides a surface fabric with effect of reflection of light night, includes basic surface course, reflection of light material layer and tie coat, and wherein, the tie coat sets up between basic surface course and reflection of light material layer, and the tie coat is modified polyurethane adhesive, and the composition of basic surface course is cotton, reflection of light material layer is the dacron cloth that is coated with phosphor coating.
The light reflecting material layer is fixed with the base fabric layer in a partial coverage mode, wherein the partial coverage means that the coverage area of the light reflecting material layer on the surface of the base fabric layer is less than 50%.
The preparation method of the modified polyurethane adhesive comprises the following steps:
s1, under the condition of room temperature, weighing N, N-dimethylformamide, placing the N, N-dimethylformamide into a three-neck flask, adding sodium hydroxide to adjust the pH to 11.0-12.0, uniformly stirring, adding ethylene glycol diglycidyl ether and 2-amino-4-hydroxy-6-methylpyrimidine, and uniformly stirring at room temperature to form an intermediate reaction solution;
wherein the mass ratio of the ethylene glycol diglycidyl ether to the 2-amino-4-hydroxy-6-methylpyrimidine to the N, N-dimethylformamide is 1.7:1.2:10.
S2, gradually heating the intermediate reaction liquid to 50 ℃, stirring the reaction liquid at the speed of 300r/min, carrying out heat preservation reaction for 3 hours, naturally cooling to room temperature, and removing the solvent to obtain the modified chain extender;
s3, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 70 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 2 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1:1; the addition amount of dibutyl tin dilaurate is 0.2% of the mass of isophorone diisocyanate.
S4, adding a modified chain extender into the prepolymerization reaction mixture, continuing to perform heat preservation reaction for 1-3 hours, then cooling to 40 ℃, adding triethylamine, performing heat preservation stirring for 10 minutes, and adding ethyl acetate to adjust the solid content to 55% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the modified chain extender to the isophorone diisocyanate in S3 is 1:5, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in S3 is 1:8.
The preparation process of the fabric with the night light reflecting effect comprises the following steps:
coating the non-reflective surface of the reflective material layer with a modified polyurethane adhesive with the sizing amount of 15g/m 2 And then bonding the base fabric layer to the part to be bonded, heating to 55 ℃, carrying out hot pressing treatment for 1min, and cooling to obtain the fabric with the night light reflection effect.
Example 3
The fabric with the night light-reflecting effect comprises a basic fabric layer, a light-reflecting material layer and a bonding layer, wherein the bonding layer is arranged between the basic fabric layer and the light-reflecting material layer, the bonding layer is a modified polyurethane adhesive, the basic fabric layer is formed by blending polyester and cotton (polyester: cotton mass ratio is 7:3), and the light-reflecting material layer is polyester fabric bonded with glass beads.
The light reflecting material layer is fixed with the base fabric layer in a partial coverage mode, wherein the partial coverage means that the coverage area of the light reflecting material layer on the surface of the base fabric layer is less than 50%.
The preparation method of the modified polyurethane adhesive comprises the following steps:
s1, under the condition of room temperature, weighing N, N-dimethylformamide, placing the N, N-dimethylformamide into a three-neck flask, adding sodium hydroxide to adjust the pH to 11.0-12.0, uniformly stirring, adding ethylene glycol diglycidyl ether and 2-amino-4-hydroxy-6-methylpyrimidine, and uniformly stirring at room temperature to form an intermediate reaction solution;
wherein the mass ratio of the ethylene glycol diglycidyl ether, the 2-amino-4-hydroxy-6-methylpyrimidine and the N, N-dimethylformamide is 3.4:2.4:20.
S2, gradually heating the intermediate reaction liquid to 60 ℃, stirring the reaction liquid at the speed of 500r/min, carrying out heat preservation reaction for 10 hours, naturally cooling to room temperature, and removing the solvent to obtain the modified chain extender;
s3, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 80 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 3 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1.2:1; the addition amount of dibutyl tin dilaurate is 0.6% of the mass of isophorone diisocyanate.
S4, adding a modified chain extender into the prepolymerization reaction mixture, continuing to perform heat preservation reaction for 3 hours, then cooling to 50 ℃, adding triethylamine, performing heat preservation stirring for 20 minutes, and adding ethyl acetate to adjust the solid content to 85% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the modified chain extender to the isophorone diisocyanate in S3 is 1:10, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in S3 is 1:16.
The preparation process of the fabric with the night light reflecting effect comprises the following steps:
coating the non-reflective surface of the reflective material layer with modified polyurethane adhesive with the sizing amount of 35g/m 2 And then bonding the base fabric layer at the position to be bonded, heating to 60 ℃, carrying out hot pressing treatment for 3min, and cooling to obtain the fabric with the night light reflection effect.
Comparative example 1
A polyurethane adhesive differs from example 1 only in that the modified chain extender is replaced by the conventional chain extender 1, 4-butanediol during the preparation of the polyurethane adhesive.
The preparation method of the polyurethane adhesive comprises the following steps:
s1, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 75 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 2 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1.1:1; the addition amount of dibutyl tin dilaurate is 0.4% of the mass of isophorone diisocyanate.
S2, adding a chain extender 1, 4-butanediol into the prepolymerization reaction mixture, continuously preserving heat and reacting for 2 hours, then cooling to 45 ℃, adding triethylamine, preserving heat and stirring for 15 minutes, and adding ethyl acetate to adjust the solid content to 75% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the chain extender to the isophorone diisocyanate in S1 is 1:8, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in S1 is 1:12.
Comparative example 2
A polyurethane adhesive differs from example 1 only in that the chain extender is replaced by ethylene glycol diglycidyl ether during the preparation of the polyurethane adhesive.
The preparation method of the polyurethane adhesive comprises the following steps:
s1, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 75 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 2 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1.1:1; the addition amount of dibutyl tin dilaurate is 0.4% of the mass of isophorone diisocyanate.
S2, adding ethylene glycol diglycidyl ether into the prepolymerization reaction mixture, continuously preserving heat for 2 hours, then cooling to 45 ℃, adding triethylamine, preserving heat and stirring for 15 minutes, and adding ethyl acetate to adjust the solid content to 75% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the ethylene glycol diglycidyl ether to the isophorone diisocyanate in S1 is 1:8, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in S1 is 1:12.
Comparative example 3
A polyurethane adhesive differs from example 1 only in that the chain extender is replaced by 2-amino-4-hydroxy-6-methylpyrimidine during the preparation of the polyurethane adhesive.
The preparation method of the polyurethane adhesive comprises the following steps:
s1, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 75 ℃, introducing nitrogen as a protective gas, sequentially adding isophorone diisocyanate and dibutyltin dilaurate, and carrying out heat preservation reaction for 2 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
wherein the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1.1:1; the addition amount of dibutyl tin dilaurate is 0.4% of the mass of isophorone diisocyanate.
S2, adding 2-amino-4-hydroxy-6-methylpyrimidine into the prepolymerization reaction mixture, continuously preserving heat for 2 hours, then cooling to 45 ℃, adding triethylamine, preserving heat, stirring for 15 minutes, and adding ethyl acetate to adjust the solid content to 75% after the reaction is finished, thus obtaining the modified polyurethane adhesive;
wherein the mass ratio of the addition amount of the 2-amino-4-hydroxy-6-methylpyrimidine to the isophorone diisocyanate in the S1 is 1:8, and the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in the S1 is 1:12.
Experimental example
The invention performs performance detection and comparison on the modified polyurethane adhesive or polyurethane adhesive prepared in the example 1 and the comparative examples 1-3, and the detection is that the peeling strength between two layers of polyester fabrics (polyester fiber fineness: 1.67dtex, warp density: 86 roots/inch, weft density: 72 roots/inch).
The detection comprises the following steps:
(1) The detection of the peel strength is referred to GB/T2792-2014;
(2) Washing with JIS L0217-103 washing detection standard, washing times of 30 times at 40deg.C for 20min each time; the water washing is to use pure tap water for washing; the chemical washing is washing by tap water containing chemical detergent, wherein the chemical detergent is sodium fatty alcohol polyoxyethylene ether sulfate (AES) with the mass concentration of 1%;
(3) The heat aging resistance was measured by placing at 25℃at 50RH% for 48 hours, then at 50℃at 50RH% for 120 hours, and finally at 25℃at 50RH% for 30 minutes, and the peel strength and yellowing degree were measured, and the yellowing degree was classified into 0 (no yellowing at all), 1 (slight yellowing), 2 (slight yellowing), 3 (moderate yellowing) and 4 (severe yellowing) as the level was higher.
The bonding results are shown in table 1.
TABLE 1 Performance of different Adhesives
As can be seen from the test data in table 1, the adhesive prepared in example 1 has higher initial peel strength, and better performances of water washing resistance, chemical washing resistance and aging resistance than the corresponding comparative examples, which indicates that the fabric with the night light reflecting effect prepared by using the adhesive of example 1 of the invention is less prone to falling off and yellowing and is more durable.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (8)

1. The fabric with the night light-reflecting effect is characterized by comprising a basic fabric layer, a light-reflecting material layer and a bonding layer, wherein the bonding layer is arranged between the basic fabric layer and the light-reflecting material layer, the bonding layer is a modified polyurethane adhesive, and the modified polyurethane adhesive is synthesized under the action of a modified chain extender by using isophorone diisocyanate and polycarbonate diol as reactants;
the preparation method of the modified polyurethane adhesive comprises the following steps:
s1, under the condition of room temperature, weighing N, N-dimethylformamide, placing the N, N-dimethylformamide into a three-neck flask, adding sodium hydroxide to adjust the pH to 11.0-12.0, uniformly stirring, adding ethylene glycol diglycidyl ether and 2-amino-4-hydroxy-6-methylpyrimidine, and uniformly stirring at room temperature to form an intermediate reaction solution;
s2, gradually heating the intermediate reaction liquid to 50-60 ℃, stirring the reaction liquid at a speed of 300-500r/min, carrying out heat preservation reaction for 3-10h, naturally cooling to room temperature, and removing the solvent to obtain the modified chain extender;
s3, firstly taking polycarbonate diol, carrying out vacuum dehydration treatment for 2 hours at 120 ℃, then cooling to 70-80 ℃, introducing nitrogen as a shielding gas, sequentially adding isophorone diisocyanate and a catalyst, and carrying out heat preservation reaction for 2-3 hours to complete a prepolymerization reaction to obtain a prepolymerization reaction mixture;
s4, adding a modified chain extender into the prepolymerization reaction mixture, continuing to perform heat preservation reaction for 1-3 hours, then cooling to 40-50 ℃, adding triethylamine, performing heat preservation stirring for 10-20 minutes, and adding ethyl acetate to adjust the solid content after the reaction is finished, thus obtaining the modified polyurethane adhesive;
in the S1, the mass ratio of the ethylene glycol diglycidyl ether, the 2-amino-4-hydroxy-6-methylpyrimidine and the N, N-dimethylformamide is 1.7-3.4:1.2-2.4:10-20.
2. The fabric with the night light reflecting effect according to claim 1, wherein the component of the basic fabric layer is any one of polyester, cotton, hemp, polyester-cotton blending, polyester-hemp blending and cotton-hemp blending.
3. The fabric with the night light reflecting effect according to claim 1, wherein the light reflecting material layer is a fabric adhered with glass beads or a fabric coated with phosphorescent paint.
4. The fabric with night light reflecting effect according to claim 1, wherein the light reflecting material layer is fixed with the base fabric layer in a partially covered manner, wherein the partially covered means that the coverage area of the light reflecting material layer on the surface of the base fabric layer is less than 50%.
5. The fabric with the night light reflecting effect according to claim 1, wherein in the step S3, the molecular weight of the polycarbonate diol is 2000, and the molar ratio of isophorone diisocyanate to the polycarbonate diol is 1-1.2:1; the catalyst is dibutyl tin dilaurate, and the addition amount is 0.2-0.6% of the mass of isophorone diisocyanate.
6. The fabric with the night light reflecting effect according to claim 1, wherein the mass ratio of the addition amount of the modified chain extender to the isophorone diisocyanate in S3 in S4 is 1:5-10; the mass ratio of the addition amount of the triethylamine to the isophorone diisocyanate in the S3 is 1:8-16; the solid content of the modified polyurethane adhesive is 55% -85%.
7. A process for preparing a fabric with a night light reflecting effect as claimed in claim 1, which is characterized by comprising the following steps:
coating a modified polyurethane adhesive on the non-reflective surface of the reflective material layer, then bonding the surface to the part of the basic fabric layer to be bonded, heating to 55-60 ℃, carrying out hot pressing treatment for 1-3min, and cooling to obtain the fabric with the night reflective effect.
8. The process for preparing a fabric with night light reflecting effect according to claim 7, wherein the process comprises the following steps ofThe sizing amount of the modified polyurethane adhesive on the reflecting material layer is 15-35g/m 2 。
CN202310841684.7A 2023-07-11 2023-07-11 Fabric with night light reflecting effect and preparation process Active CN116552063B (en)

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Publication number Priority date Publication date Assignee Title
US4931487A (en) * 1988-03-04 1990-06-05 Dow Chemical Company Chain extenders for polyurethanes
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CN115417965A (en) * 2022-10-09 2022-12-02 中国科学院兰州化学物理研究所 Telechelic polyurethane and preparation method and application thereof
CN116003730A (en) * 2023-01-10 2023-04-25 东华大学 Self-repairing polyurethane material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4931487A (en) * 1988-03-04 1990-06-05 Dow Chemical Company Chain extenders for polyurethanes
CN1746251A (en) * 2005-09-14 2006-03-15 北京高盟化工有限公司 Special binder of reflecting material and production thereof
CN115417965A (en) * 2022-10-09 2022-12-02 中国科学院兰州化学物理研究所 Telechelic polyurethane and preparation method and application thereof
CN116003730A (en) * 2023-01-10 2023-04-25 东华大学 Self-repairing polyurethane material

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