CN111515109B - Process for making washing-resistant high-brightness color reflecting product - Google Patents

Process for making washing-resistant high-brightness color reflecting product Download PDF

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CN111515109B
CN111515109B CN202010344897.5A CN202010344897A CN111515109B CN 111515109 B CN111515109 B CN 111515109B CN 202010344897 A CN202010344897 A CN 202010344897A CN 111515109 B CN111515109 B CN 111515109B
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layer
resin
micro
color
adhesive
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CN111515109A (en
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孙飞
王小宝
胡锋
张思哲
王晨
郭育民
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Zhejiang Longyou Daoming Optics & Chemical Co ltd
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Zhejiang Longyou Daoming Optics & Chemical Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/56—Three layers or more
    • B05D7/58—No clear coat specified
    • 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
    • B32B37/02—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
    • 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
    • B32B37/1284—Application of adhesive
    • 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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/10—Removing layers, or parts of layers, mechanically or chemically
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694—Halides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2503/00—Polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2507/00—Polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2508/00—Polyesters
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/402—Coloured
    • B32B2307/4026—Coloured within the layer by addition of a colorant, e.g. pigments, dyes
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/402—Coloured
    • B32B2307/404—Multi-coloured
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/416—Reflective
    • 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
    • B32B2437/00—Clothing

Abstract

The invention discloses a process for manufacturing a washing-resistant high-brightness color reflective product, which comprises the following steps: (a) forming a bead planting film; (b) adding solid hard saturated polyester, unsaturated polyester soft resin, carboxyl-terminated polyolefin resin and a solvent A into a reaction kettle to prepare mixed resin A; (c) adding the mixed resin B, the metal complex dye and the solvent B into a stirrer to prepare colored resin; (d) coating color resin on the bead planting film to form a color resin layer; (e) forming a reflective layer on the color resin layer; (f) preparing an adhesive by taking a curing agent and mixing the resin A; (g) coating an adhesive on the reflecting layer to obtain an adhesive layer; (h) and compounding the adhesive layer and the base material layer, and stripping the carrier to form the glass bead layer to obtain the washing-resistant high-brightness colorful reflective product. By adopting the process steps, the production efficiency can be greatly improved, and the prepared highlight color reflective product has the advantages of washing resistance, uniform and bright color, excellent retroreflective effect and the like.

Description

Process for making washing-resistant high-brightness color reflecting product
Technical Field
The invention relates to the field of reflective materials, in particular to a manufacturing process of a washing-resistant high-brightness colored reflective product.
Background
The highlight color reflective product is usually an exposed glass bead reflective product, so that the color is bright, the highlight color reflective product is generally used for civil clothing or fashionable dress, the colorization and fashion requirements of the fashionable dress can be met, and meanwhile, the highlight color reflective product also can play a role in safety protection of a wearer to a certain extent.
However, the bright color retroreflective articles in the prior art hardly meet the requirement of the retroreflective factor of the conventional retroreflective articles, and because the bright color retroreflective articles have certain requirements on the washing resistance of the bright color retroreflective articles when being used in civil clothing or fashion, the bright color retroreflective articles generally require not less than 25 times in the case of household washing, but generally have longer service life when the washing resistance is more.
However, the conventional polyurethane or acrylic resin is generally used as the main resin in the production of the existing high-brightness color reflective product, so that the obtained high-brightness color reflective product has poor washing resistance. The glass beads in the existing highlight color reflective product have larger particle size difference and wider distribution, so that the adhesive in the highlight color reflective product has poorer wrapping property on the glass beads with larger particle size, and the glass beads with larger particle size are easy to fall off in the washing process, thereby causing the poor washing resistance of the existing highlight color reflective product.
In addition, patent document CN101380834A discloses a preparation process of highlight color reflective fabric, wherein the preparation process disclosed in the patent document refers to a production speed of 2-5 m/min, and the problem of low production efficiency of the existing preparation process is known.
In view of the above problems, the present process for manufacturing a high-brightness color reflective product is still to be improved.
Disclosure of Invention
The invention provides a novel manufacturing process of washing-resistant highlight color reflective products, aiming at the defects of poor washing resistance, low production efficiency and the like of the highlight color reflective products in the prior art.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the manufacturing process of the washing-resistant high-brightness colored reflective product comprises a glass bead layer, a colored resin layer, a reflective layer, an adhesive layer and a base material layer, wherein the thickness of the adhesive layer is 30-120 mu m, the thickness of the colored resin layer is 2-10 mu m, the thickness of the reflective layer is 15-40 nm, and the manufacturing steps are as follows:
(a) placing a carrier and glass beads in bead planting equipment, uniformly arranging the glass beads on the surface of the carrier by adopting a gluing or heating mode to form a bead planting film, wherein the glass beads are arranged in a single layer and have a particle size error within 10 mu m;
(b) adding solid hard saturated polyester and unsaturated polyester soft resin into a reaction kettle to serve as main resin, wherein the glass transition temperature Tg of the solid hard saturated polyester is 40-80 ℃, the molecular weight is 20000-60000, the hydroxyl value is 10-30 mgKOH/g, the glass transition temperature Tg of the unsaturated polyester soft resin is-4-20 ℃, the molecular weight is 40000-80000, and the hydroxyl value is 2-6 mgKOH/g, adding carboxyl-terminated polyolefin resin into the reaction kettle to serve as auxiliary resin, and further adding a solvent A, wherein the solid hard saturated polyester, the unsaturated polyester soft resin, the polyolefin resin and the solvent A are prepared according to the mass ratio of 1:0.2:0.05: 0.6-1: 0.8:0.15:2, then heating the reaction kettle to 50-80 ℃, stirring for 120-300 min, and cooling to obtain mixed resin A;
(c) adding mixed resin B, metal complex dye and solvent B into a stirrer, wherein the mixed resin B is one or a mixture of polyester resin, polyurethane resin or epoxy modified polyurethane resin, the mixed resin B, the metal complex dye and the solvent B are prepared according to the mass part ratio of 100:8: 80-100: 40:300, and stirring the components at room temperature for 15-45 min to obtain color resin;
(d) uniformly coating the color resin on the bead planting film by adopting a micro-concave coating device to form a uniform color resin layer, wherein the number of the reticulate lines of a micro-concave roller of the micro-concave coating device is 20-200 lines, the rotating speed of the micro-concave roller is 20-150 m/min, and the ratio of the surface linear speed of the micro-concave roller to the linear speed of a coating is 1: 0.8-1: 2;
(e) carrying out vapor deposition on the surface of the color resin layer by adopting a vacuum evaporation method or a magnetron sputtering method to form the reflecting layer, wherein the reflecting layer is a total reflecting layer or a semi-reflecting layer;
(f) adding a curing agent and the mixed resin A into a reaction kettle, wherein the curing agent is an isocyanate curing agent or an amino curing agent, the mixed resin A and the curing agent are prepared according to the mass part ratio of 100: 3-100: 20, heating the reaction kettle to 50-80 ℃, stirring for 30-150 min, and cooling to obtain an adhesive;
(g) uniformly coating the adhesive on the surface of the reflecting layer by using a precision coating machine, preparing the adhesive layer after coating, and drying for 2-5 min at the temperature of 50-140 ℃;
(h) taking a substrate layer, compounding the adhesive layer and the substrate layer by adopting compounding equipment, setting the thermal compounding temperature to be 70-130 ℃ and the compounding line pressure to be 0.3-0.8 MPa, curing and preserving for 24-120 h at 50-100 ℃ after compounding is finished, stripping a carrier on a bead planting film after curing and preserving are finished so as to form a glass bead layer, and finally preparing the washing-resistant high-brightness color reflective product.
In the step (a), the carrier is selected as a support layer of the glass beads to play a role in fixing the glass beads, and the glass beads are uniformly distributed on the surface of the carrier in a mode of directly heating and softening the carrier or coating glue on the carrier, wherein the carrier can be selected from a PET material with good mechanical property. In addition, the invention strictly controls the particle size error of the glass beads, and can ensure the arrangement regularity of the glass beads on the carrier, thereby improving the uniformity of the color, improving the retention rate of the washed glass beads, and improving the washing resistance of the obtained washing-resistant highlight color reflective product.
In the step (b), the hard segment resin of solid hard saturated polyester and the soft segment resin of unsaturated polyester soft resin are selected as the components of the mixed resin A in a proper proportion, so that a stronger chemical chain can be formed, and the higher the proportion of the hard segment resin of the solid hard saturated polyester is, the higher the hardness of the formed film layer is, and the higher the elastic modulus and the tensile strength are. The selected carboxyl-terminated polyolefin resin has the function of washing resistance auxiliary agent, so that the molecular structure of the mixed resin A is integrated, the cohesive strength and toughness are improved, and the washing resistance is obviously improved. Wherein the carboxyl-terminated polyolefin resin can be carboxyl-terminated polyolefin resin produced by krasol company, and the solvent A can be ethyl acetate or ketone solvent.
In the step (c), the color resin prepared by the raw materials has the advantages of good stability, uniform color and the like. Wherein the solvent B can be ketone solvent.
In the step (d), the reverse micro-concave coating process can not only obtain a uniform and compact coating, but also greatly improve the coating efficiency. Under the condition of the rotating speed ratio, the efficiency of the reverse micro-concave coating is high and the coating is more uniform.
In the step (e), the reflecting layer is prepared by adopting a vacuum evaporation or magnetron sputtering process, so that not only can a compact and uniform film layer be obtained, but also the thickness of the film layer can be accurately controlled.
In the step (f), the isocyanate curing agent or the amino curing agent is selected as one of the components of the adhesive, so that the adhesive has better flexibility and adhesive force, wherein the isocyanate curing agent can react with amino groups and other groups to form crosslinking, the stability of the adhesive can be effectively improved, the reaction speed of the amino curing agent is higher, and the production efficiency can be improved.
In the step (g) and the step (h), the mixed resin A and the curing agent are fully reacted through coating and thermal compounding processes, and the mixed resin A is heated at a stepped temperature and cured for a long time to ensure that the solvent A is completely volatilized.
By adopting the process steps, the production efficiency can be greatly improved, and the finally prepared highlight color reflective product has the advantages of washing resistance, uniform and bright color, excellent retroreflective effect and the like.
Preferably, in the above process for manufacturing a washing-resistant bright color reflective product, in the step (e), the total reflection layer is an aluminum layer or a silver layer.
The total reflection layer formed by the aluminum layer or the silver layer has excellent retroreflection performance, so that the finally prepared retroreflective article has excellent retroreflection performance, and the coefficient of retroreflection exceeds 400 cd/lx-m2。
Preferably, in the above process for manufacturing a washing-resistant bright color reflective article, in step (e), the semi-reflective layer is a single layer film made of zinc sulfide or magnesium fluoride.
The single-layer semi-reflecting layer composed of zinc sulfide or magnesium fluoride has high transparency, so that the finally prepared reflecting product has bright and high bright color.
Preferably, in the above manufacturing process of the washing-resistant bright colored reflective product, in the step (e), the semi-reflective layer is a multilayer film composed of zinc sulfide or magnesium fluoride.
The multilayer semi-reflective layer composed of zinc sulfide or magnesium fluoride has high transparency, so that the finally prepared reflective product has bright and high bright color.
Preferably, in the above process for manufacturing the washing-resistant high-brightness color reflective product, in the step (d), the rotation speed of the micro-concave roller is 40-100 m/min.
If the coating speed of the micro-concave reverse coating is too low, the coated color layer is too thick, and the color uniformity is poor; if the coating rotation speed exceeds 100m/min, the color resin is scattered. The rotating speed range is selected, so that the uniformity and the stability of coating can be ensured.
Preferably, in the above process for manufacturing a washing-resistant high-brightness color reflective product, in the step (d), the micro-concave roller is a metal micro-concave roller or a ceramic micro-concave roller.
The manufacturing process of the metal micro-concave roller is relatively simple, the cost performance is high, the ceramic micro-concave roller is good in wear resistance, long in service life and high in production efficiency.
Preferably, in the process for manufacturing the washing-resistant high-brightness colored reflective product, in the step (a), the particle size of the glass beads is 75-80 μm.
The particle size range of the glass beads is limited in the range, the error value of the particle size among the glass beads can be further controlled, the arrangement uniformity of the glass beads is further improved, and the retroreflection effect of the glass beads in the particle size range is optimal.
Preferably, in the above manufacturing process of the washing-resistant bright colored reflective article, in the step (c), the metal complex dye is an orelin metal complex dye of basf.
The dye of the austempered metal complex of Basfu has good compatibility with the solvent B and bright color.
Preferably, in the process for manufacturing the washing-resistant high-brightness colored reflective product, in the step (b), the glass transition temperature of the mixed resin A is-5 to-30 ℃, and the molecular weight of the mixed resin A is 8000 to 40000.
The glass transition temperature of the mixed resin A is controlled in a lower range, so that the prepared mixed resin A is soft, can better form a spatial three-dimensional structure with a curing agent, and improves the washing resistance.
Preferably, in the manufacturing process of the washing-resistant high-brightness colored reflective product, the material of the substrate layer is fabric, hot melt adhesive or leather base.
The material of the substrate layer has the advantages of convenient material acquisition and lower cost, and is more beneficial to preparing diversified high-brightness colored reflective products.
Compared with the prior art, the invention has the outstanding beneficial effects that:
1. the invention adopts the reverse micro-concave coating mode, which can obviously improve the production efficiency and has better coating effect than the traditional coating process;
2. the invention strictly controls the particle size of the glass beads, is beneficial to forming a uniformly arranged bead planting film, further improves the uniformity of the colored resin layer and the reflecting layer, and obviously improves the retroreflection effect of the finally prepared high-brightness colored reflecting product.
3. The mixed resin A, the mixed resin B and the adhesive prepared by the formula have excellent washing resistance, and the service life of the highlight color reflective product is remarkably prolonged.
Drawings
FIG. 1 is a schematic structural view of a highlighted colored retroreflective article prior to stripping the carrier;
FIG. 2 is a schematic structural diagram of a launderable highlight-resistant colored retroreflective article made in accordance with the present invention;
fig. 3 is a partially enlarged view of a portion a in fig. 2.
Detailed Description
The invention will be described in further detail below with reference to the accompanying figures 1-3 and the detailed description, but they are not intended to limit the invention:
example 1
A manufacturing process of a washing-resistant high-brightness colored reflective product comprises a glass bead layer 1, a colored resin layer 2, a reflective layer 3, an adhesive layer 4 and a base material layer 5, wherein the thickness of the adhesive layer 4 is 30 micrometers, the thickness of the colored resin layer 2 is 2 micrometers, the thickness of the reflective layer 3 is 15nm, and the manufacturing steps are as follows:
(a) placing a carrier 6 and glass beads 11 in bead planting equipment, uniformly arranging the glass beads 11 on the surface of the carrier 6 by adopting a gluing or heating mode to form a bead planting film 7, wherein the glass beads 11 are arranged in a single layer and have a particle size error within 10 micrometers;
(b) adding solid hard saturated polyester and unsaturated polyester soft resin into a reaction kettle to serve as main resin, wherein the glass transition temperature Tg of the solid hard saturated polyester is 40 ℃, the molecular weight is 20000, and the hydroxyl value is 10mgKOH/g, the glass transition temperature Tg of the unsaturated polyester soft resin is-4 ℃, the molecular weight is 40000, and the hydroxyl value is 2mgKOH/g, adding carboxyl-terminated polyolefin resin into the reaction kettle to serve as auxiliary resin, and continuously adding a solvent A, wherein the solid hard saturated polyester, the unsaturated polyester soft resin, the polyolefin resin and the solvent A are prepared according to the mass part ratio of 1:0.2:0.05:0.6, then heating the reaction kettle to 50 ℃, stirring for 120min, and cooling to obtain mixed resin A;
(c) adding mixed resin B, metal complex dye and solvent B into a stirrer, wherein the mixed resin B is one or a mixture of polyester resin, polyurethane resin or epoxy modified polyurethane resin, the mixed resin B, the metal complex dye and the solvent B are prepared according to the mass part ratio of 100:8:80, and stirring the components for 15min at room temperature to prepare color resin;
(d) uniformly coating the color resin on the bead planting film 7 by using a micro-concave coating device to form a uniform color resin layer 2, wherein the number of the reticulate lines of a micro-concave roller of the micro-concave coating device is 20 lines, the rotating speed of the micro-concave roller is 20m/min, and the ratio of the surface linear speed of the micro-concave roller to the coating linear speed is 1: 0.8;
(e) performing vapor deposition on the surface of the color resin layer 2 by adopting a vacuum evaporation method or a magnetron sputtering method to form the reflecting layer 3, wherein the reflecting layer 3 is a total reflecting layer or a semi-reflecting layer;
(f) adding a curing agent and the mixed resin A into a reaction kettle, wherein the curing agent is an isocyanate curing agent or an amino curing agent, the mixed resin A and the curing agent are prepared according to the mass part ratio of 100:3, heating the reaction kettle to 50 ℃, stirring for 30min, and cooling to obtain an adhesive;
(g) uniformly coating the adhesive on the surface of the reflecting layer 3 by using a precision coating machine, preparing the adhesive layer 4 after coating, and drying for 2min at the temperature of 50 ℃;
(h) taking a substrate layer 5, compounding the adhesive layer 4 and the substrate layer 5 by adopting compounding equipment, setting the thermal compounding temperature to be 70 ℃ and the compounding line pressure to be 0.3MPa, curing and curing at 50 ℃ for 24 hours after compounding, stripping the carrier 6 on the bead planting film 7 after curing and curing is finished so as to form a glass bead layer 1, and finally preparing the washing-resistant high-brightness color reflective product.
Preferably, in the step (e), the total reflection layer is an aluminum layer or a silver layer.
Preferably, in the step (e), the semi-reflective layer is a single layer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (e), the semi-reflective layer is a multilayer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (d), the rotation speed of the micro-concave roller is 40 m/min.
Preferably, in the step (d), the micro-concave roller is a metal micro-concave roller or a ceramic micro-concave roller.
Preferably, in the step (a), the particle size of the glass beads 11 is 75 to 80 μm.
Preferably, in the step (c), the metal complex dye is an orexin metal complex dye of basf.
Preferably, in the step (b), the glass transition temperature of the mixed resin A is-5 ℃ and the molecular weight is 8000.
Preferably, the material of the substrate layer 5 is fabric, hot melt adhesive or leather base.
Example 2
A manufacturing process of a washing-resistant high-brightness colored reflective product comprises a glass bead layer 1, a colored resin layer 2, a reflective layer 3, an adhesive layer 4 and a base material layer 5, wherein the thickness of the adhesive layer 4 is 120 micrometers, the thickness of the colored resin layer 2 is 10 micrometers, the thickness of the reflective layer 3 is 40nm, and the manufacturing steps are as follows:
(a) placing a carrier 6 and glass beads 11 in bead planting equipment, uniformly arranging the glass beads 11 on the surface of the carrier 6 by adopting a gluing or heating mode to form a bead planting film 7, wherein the glass beads 11 are arranged in a single layer and have a particle size error within 10 micrometers;
(b) adding solid hard saturated polyester and unsaturated polyester soft resin into a reaction kettle to serve as main resin, wherein the glass transition temperature Tg of the solid hard saturated polyester is 80 ℃, the molecular weight is 60000 and the hydroxyl value is 30mgKOH/g, the glass transition temperature Tg of the unsaturated polyester soft resin is-20 ℃, the molecular weight is 80000 and the hydroxyl value is 6mgKOH/g, adding carboxyl-terminated polyolefin resin into the reaction kettle to serve as auxiliary resin, and continuously adding a solvent A, wherein the solid hard saturated polyester, the unsaturated polyester soft resin, the polyolefin resin and the solvent A are prepared according to the mass part ratio of 1:0.8:0.15:2, heating the reaction kettle to 80 ℃, stirring for 300min, and cooling to obtain mixed resin A;
(c) adding mixed resin B, metal complex dye and solvent B into a stirrer, wherein the mixed resin B is one or a mixture of polyester resin, polyurethane resin or epoxy modified polyurethane resin, the mixed resin B, the metal complex dye and the solvent B are prepared according to the mass part ratio of 100:40:300, and stirring the components for 45min at room temperature to prepare color resin;
(d) uniformly coating the color resin on the bead planting film 7 by using a micro-concave coating device to form a uniform color resin layer 2, wherein the number of the reticulate lines of a micro-concave roller of the micro-concave coating device is 200 lines, the rotating speed of the micro-concave roller is 150m/min, and the ratio of the surface linear speed of the micro-concave roller to the coating linear speed is 1: 2;
(e) performing vapor deposition on the surface of the color resin layer 2 by adopting a vacuum evaporation method or a magnetron sputtering method to form the reflecting layer 3, wherein the reflecting layer 3 is a total reflecting layer or a semi-reflecting layer;
(f) adding a curing agent and the mixed resin A into a reaction kettle, wherein the curing agent is an isocyanate curing agent or an amino curing agent, the mixed resin A and the curing agent are prepared according to the mass part ratio of 100:20, heating the reaction kettle to 80 ℃, stirring for 150min, and cooling to obtain an adhesive;
(g) uniformly coating the adhesive on the surface of the reflecting layer 3 by using a precision coating machine, preparing the adhesive layer 4 after coating, and drying for 5min at 140 ℃;
(h) taking a substrate layer 5, compounding the adhesive layer 4 and the substrate layer 5 by adopting compounding equipment, setting the thermal compounding temperature at 130 ℃ and the compounding line pressure at 0.8MPa, curing and maintaining the substrate layer at 100 ℃ for 120h after the compounding is finished, stripping the carrier 6 on the bead planting film 7 after the curing and maintaining are finished so as to form a glass bead layer 1, and finally preparing the washing-resistant high-brightness color reflective product.
Preferably, in the step (e), the total reflection layer is an aluminum layer or a silver layer.
Preferably, in the step (e), the semi-reflective layer is a single layer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (e), the semi-reflective layer is a multilayer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (d), the rotation speed of the micro-concave roller is 100 m/min.
Preferably, in the step (d), the micro-concave roller is a metal micro-concave roller or a ceramic micro-concave roller.
Preferably, in the step (a), the particle size of the glass beads 11 is 75 to 80 μm.
Preferably, in the step (c), the metal complex dye is an orexin metal complex dye of basf.
Preferably, in the step (b), the glass transition temperature of the mixed resin A is-30 ℃ and the molecular weight is 40000.
Preferably, the material of the substrate layer 5 is fabric, hot melt adhesive or leather base.
Example 3
A manufacturing process of a washing-resistant high-brightness colored reflective product comprises a glass bead layer 1, a colored resin layer 2, a reflective layer 3, an adhesive layer 4 and a base material layer 5, wherein the thickness of the adhesive layer 4 is 50 micrometers, the thickness of the colored resin layer 2 is 6 micrometers, the thickness of the reflective layer 3 is 27nm, and the manufacturing steps are as follows:
(a) placing a carrier 6 and glass beads 11 in bead planting equipment, uniformly arranging the glass beads 11 on the surface of the carrier 6 by adopting a gluing or heating mode to form a bead planting film 7, wherein the glass beads 11 are arranged in a single layer and have a particle size error within 10 micrometers;
(b) adding solid hard saturated polyester and unsaturated polyester soft resin into a reaction kettle to serve as main resin, wherein the glass transition temperature Tg of the solid hard saturated polyester is 60 ℃, the molecular weight is 40000, and the hydroxyl value is 20mgKOH/g, the glass transition temperature Tg of the unsaturated polyester soft resin is-18 ℃, the molecular weight is 60000, and the hydroxyl value is 4mgKOH/g, adding carboxyl-terminated polyolefin resin into the reaction kettle to serve as auxiliary resin, and continuously adding a solvent A, wherein the solid hard saturated polyester, the unsaturated polyester soft resin, the polyolefin resin, and the solvent A are prepared according to the mass part ratio of 1:0.5:0.1:1.3, then heating the reaction kettle to 65 ℃, stirring for 210min, and cooling to obtain mixed resin A;
(c) adding mixed resin B, metal complex dye and solvent B into a stirrer, wherein the mixed resin B is one or a mixture of polyester resin, polyurethane resin or epoxy modified polyurethane resin, the mixed resin B, the metal complex dye and the solvent B are prepared according to the mass part ratio of 100:24:190, and stirring the components for 30min at room temperature to prepare color resin;
(d) uniformly coating the color resin on the bead planting film 7 by using a micro-concave coating device to form a uniform color resin layer 2, wherein the mesh line number of a micro-concave roller of the micro-concave coating device is 110 lines, the rotating speed of the micro-concave roller is 80m/min, and the ratio of the surface linear speed of the micro-concave roller to the coating linear speed is 1: 1.2;
(e) performing vapor deposition on the surface of the color resin layer 2 by adopting a vacuum evaporation method or a magnetron sputtering method to form the reflecting layer 3, wherein the reflecting layer 3 is a total reflecting layer or a semi-reflecting layer;
(f) adding a curing agent and the mixed resin A into a reaction kettle, wherein the curing agent is an isocyanate curing agent or an amino curing agent, the mixed resin A and the curing agent are prepared according to the mass part ratio of 100:12, heating the reaction kettle to 65 ℃, stirring for 90min, and cooling to obtain an adhesive;
(g) uniformly coating the adhesive on the surface of the reflecting layer 3 by using a precision coating machine, preparing the adhesive layer 4 after coating, and drying for 3min at the temperature of 100 ℃;
(h) taking a substrate layer 5, compounding the adhesive layer 4 and the substrate layer 5 by adopting compounding equipment, setting the thermal compounding temperature to be 100 ℃ and the compounding line pressure to be 0.5MPa, curing and curing at 80 ℃ for 72h after compounding, stripping the carrier 6 on the bead-planted film 7 after curing and curing is finished so as to form the glass bead layer 1, and finally preparing the washing-resistant high-brightness color reflective product.
Preferably, in the step (e), the total reflection layer is an aluminum layer or a silver layer.
Preferably, in the step (e), the semi-reflective layer is a single layer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (e), the semi-reflective layer is a multilayer film composed of zinc sulfide or magnesium fluoride.
Preferably, in the step (d), the rotation speed of the micro-concave roller is 70 m/min.
Preferably, in the step (d), the micro-concave roller is a metal micro-concave roller or a ceramic micro-concave roller.
Preferably, in the step (a), the particle size of the glass beads 11 is 75 to 80 μm.
Preferably, in the step (c), the metal complex dye is an orexin metal complex dye of basf.
Preferably, in the step (b), the glass transition temperature of the mixed resin A is-17 ℃ and the molecular weight is 24000.
Preferably, the material of the substrate layer 5 is fabric, hot melt adhesive or leather base.
Example 4
Taking the reflective products obtained in the above examples, taking the commercially available high-brightness color reflective product of CSR-H1008 model, the high-brightness color reflective product of SMGC2100 model and the high-brightness color reflective product of 8712NCOM-1013 model as comparative examples, carrying out the tests of two performances of the retroreflective coefficient and the washing resistance, wherein the test method is as follows:
firstly, testing the retroreflection coefficient: the initial coefficient of retroreflection of the samples was tested as specified in GB 20653;
secondly, washing resistance testing: the coefficient of retroreflection of the samples after 75 cycles of washing was tested as specified in GB/T86296N;
the performance parameters of the retroreflective articles and comparative examples obtained in the examples of the present invention are shown in Table 1:
TABLE 1
Figure BDA0002469716230000101
Wherein comparative example 1 is a CSR-H1008 model highlight color retroreflective article, comparative example 2 is an SMGC2100 model highlight color retroreflective article, and comparative example 3 is a 8712NCOM-1013 model highlight color retroreflective article.
In summary, the above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the present invention.

Claims (9)

1. The utility model provides a manufacturing technology of colour reflection of light goods of washable highlight, includes glass bead layer (1), colored resin layer (2), reflection stratum (3), gluing agent layer (4), substrate layer (5), its characterized in that: the thickness of the adhesive layer (4) is 30-120 mu m, the thickness of the colored resin layer (2) is 2-10 mu m, the thickness of the reflecting layer (3) is 15-40 nm, and the manufacturing steps are as follows:
(a) placing a carrier (6) and glass beads (11) in bead planting equipment, uniformly arranging the glass beads (11) on the surface of the carrier (6) by adopting a gluing or heating mode to form a bead planting film (7), wherein the glass beads (11) are arranged in a single layer and have a particle size error within 10 mu m;
(b) adding solid hard saturated polyester and unsaturated polyester soft resin into a reaction kettle as main resin, wherein the glass transition temperature Tg of the solid hard saturated polyester is 40-80 ℃, the molecular weight is 20000-60000, the hydroxyl value is 10-30 mgKOH/g, the glass transition temperature Tg of the unsaturated polyester soft resin is-4-20 ℃, the molecular weight is 40000-80000, and the hydroxyl value is 2-6 mgKOH/g, adding carboxyl-terminated polyolefin resin into the reaction kettle as auxiliary resin, further adding a solvent A, wherein the solid hard saturated polyester, the unsaturated polyester soft resin, the polyolefin resin and the solvent A are prepared according to the mass ratio of 1:0.2:0.05: 0.6-1: 0.8:0.15:2, then heating the reaction kettle to 50-80 ℃, stirring for 120-300 min, cooling to obtain a mixed resin A, and the glass transition temperature of the mixed resin A is-5-30 ℃, the molecular weight is 8000-40000;
(c) adding mixed resin B, metal complex dye and solvent B into a stirrer, wherein the mixed resin B is one or a mixture of polyester resin, polyurethane resin or epoxy modified polyurethane resin, the mixed resin B, the metal complex dye and the solvent B are prepared according to the mass part ratio of 100:8: 80-100: 40:300, and stirring the components at room temperature for 15-45 min to obtain color resin;
(d) uniformly coating the color resin on the bead planting film (7) by adopting a micro-concave coating device to form a uniform color resin layer (2), wherein the number of the reticulate lines of a micro-concave roller of the micro-concave coating device is 20-200 lines, the rotating speed of the micro-concave roller is 20-150 m/min, and the ratio of the surface linear speed of the micro-concave roller to the coating linear speed is 1: 0.8-1: 2;
(e) carrying out vapor deposition on the surface of the colored resin layer (2) by adopting a vacuum evaporation method or a magnetron sputtering method to form the reflecting layer (3), wherein the reflecting layer (3) is a total reflecting layer or a semi-reflecting layer;
(f) adding a curing agent and the mixed resin A into a reaction kettle, wherein the curing agent is an isocyanate curing agent or an amino curing agent, the mixed resin A and the curing agent are prepared according to the mass part ratio of 100: 3-100: 20, heating the reaction kettle to 50-80 ℃, stirring for 30-150 min, and cooling to obtain an adhesive;
(g) uniformly coating the adhesive on the surface of the reflecting layer (3) by using a precision coating machine, preparing the adhesive layer (4) after coating, and drying for 2-5 min at the temperature of 50-140 ℃;
(h) taking a substrate layer (5), compounding the adhesive layer (4) and the substrate layer (5) by adopting compounding equipment, setting the thermal compounding temperature to be 70-130 ℃ and the compounding line pressure to be 0.3-0.8 MPa, curing and curing for 24-120 h at 50-100 ℃ after compounding is finished, stripping a carrier (6) on a bead planting film (7) after curing and curing is finished so as to form a glass bead layer (1), and finally preparing the washing-resistant high-brightness color reflective product.
2. The process of claim 1, wherein the process comprises the steps of: in the step (e), the total reflection layer is an aluminum layer or a silver layer.
3. The process of claim 1, wherein the process comprises the steps of: in the step (e), the semi-reflective layer is a single-layer film composed of zinc sulfide or magnesium fluoride.
4. The process of claim 1, wherein the process comprises the steps of: in the step (e), the semi-reflective layer is a multilayer film composed of zinc sulfide or magnesium fluoride.
5. The process of claim 1, wherein the process comprises the steps of: in the step (d), the rotating speed of the micro-concave roller is 40-100 m/min.
6. The process of claim 1, wherein the process comprises the steps of: in the step (d), the micro-concave roller is a metal micro-concave roller or a ceramic micro-concave roller.
7. The process of claim 1, wherein the process comprises the steps of: in the step (a), the particle size of the glass beads (11) is 75-80 μm.
8. The process of claim 1, wherein the process comprises the steps of: in the step (c), the metal complex dye is an orexin metal complex dye of basf.
9. The process of claim 1, wherein the process comprises the steps of: the material of the substrate layer (5) is fabric or hot melt adhesive or leather base.
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