CN115260930A - Production process of super-soft reflective fabric - Google Patents
Production process of super-soft reflective fabric Download PDFInfo
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- CN115260930A CN115260930A CN202210862168.8A CN202210862168A CN115260930A CN 115260930 A CN115260930 A CN 115260930A CN 202210862168 A CN202210862168 A CN 202210862168A CN 115260930 A CN115260930 A CN 115260930A
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- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1812—C12-(meth)acrylate, e.g. lauryl (meth)acrylate
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/50—Additional features of adhesives in the form of films or foils characterized by process specific features
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/52—PV systems with concentrators
Abstract
The invention relates to the technical field of reflective materials, and provides a production process of an ultra-soft reflective fabric, which solves the problem that the existing reflective fabric is poor in softness, and comprises the following steps: s1, pretreating glass beads: surface modification is carried out on the glass beads by quaternary ammonium salt, so that the surfaces of the glass beads are positively charged; s2, low-temperature electrostatic plant: plants are arranged on the surface of the PE/PET composite film through electrostatic adsorption; s3, electroplating; s4, preparing a base fabric layer: coating a layer of adhesive on a release film, drying to form dry adhesive, and then laminating the dry adhesive with nylon cloth through a hot roller to form a base cloth layer; s5, compounding: and (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
Description
Technical Field
The invention relates to the technical field of reflective materials, in particular to a production process of an ultra-soft reflective fabric.
Background
The reflective fabric has good reflective performance, can reflect the direct light in a distant place back to a luminous position, and particularly can be easily found by a driver in a night environment, so that the life safety of operators is ensured. The manufacturing principle of the reflective fabric is that the glass beads with high refractive index are coated on the surface of the fabric substrate by a coating or film coating process, so that the common fabric can reflect light rays under the irradiation of light.
The reflective fabric sold in the market at present is widely applied to garments such as coats, jackets, cotton-padded clothes, down jackets and the like besides articles such as bags, hats and shoes, and the visibility under the environment of weak light and night light is greatly improved and the fashion originality of the garment products is improved by utilizing the reflective performance of the reflective fabric.
The prior production process of the reflective fabric can refer to patent number CN201210116812.3, and discloses a manufacturing method of anti-damage reflective fabric, which comprises the following specific steps: (1) Adhering the film surfaces of a PET film and a PE film into a composite film by using an adhesive, preheating the composite film, and planting glass beads on the composite film along with the softening of the composite film; (2) Coating a layer of ultraviolet light curing transparent adhesive on the exposed surface of the glass microspheres, and coating a layer of metal foil after the ultraviolet light curing transparent adhesive is cured; (3) And embedding the glass beads with the metal foil surface into the metal adhesive composite layer, bonding the other surface of the metal adhesive composite layer with the cloth base, and stripping the composite film after the metal adhesive composite layer is cured to obtain the anti-damage reflective cloth. In the production process of the reflective cloth, the surfaces of the glass beads are directly coated with glue, the glue before curing has good fluidity, so that gaps among the glass beads are filled with the glue, the moving space is small, and the thickness of a glue layer is thick, so that the produced product is relatively hard and poor in flexibility, and has great limitation when being applied to the field of clothes with requirements on hand feeling and comfort level.
Disclosure of Invention
Therefore, aiming at the above, the invention provides a production process of an ultra-soft reflective fabric, which solves the problem that the existing reflective fabric is poor in flexibility.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a production process of an ultra-soft reflective fabric comprises the following steps:
s1, pretreating glass beads
Dissolving quaternary ammonium salt in a solvent to prepare a quaternary ammonium salt solution with the concentration of 0.5-3 wt%, adjusting the pH value of the solution to be within the range of 2.5-4.5, then adding glass beads, stirring for 40-80 min at 35-50 ℃, filtering, washing and drying to obtain glass beads with positive charges on the surface;
s2, low-temperature electrostatic plant
Under the temperature condition of 30-40 ℃, the glass beads are used for planting plants on the surface of the PE/PET composite film through electrostatic adsorption;
s3, electroplating
Electroplating the plant PE/PET composite film to coat a metal coating on the surface of the glass microsphere to form a reflecting layer, wherein the coating is not needed before electroplating;
s4, preparation of base cloth layer
Coating a layer of adhesive on the release film, drying to form dry adhesive, and then pressing the dry adhesive with nylon cloth through a hot roller to form a base cloth layer;
s5, compounding
And (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
The further improvement is that: the quaternary ammonium salt is prepared by the following method:
(1) Dissolving N, N-dimethylallylamine in dimethylformamide, adding a photoinitiator and 1,2-ethanedithiol, and irradiating by ultraviolet light to generate a mercapto-alkene click reaction to obtain an intermediate product A;
(2) Adding gamma-glycidyl ether propyl trimethoxy silane into a reactor filled with ethanol, dissolving the intermediate product A in the ethanol, slowly dripping the intermediate product A into the reactor, and stirring and reacting for 8-20 h at 25-45 ℃ to obtain an intermediate product B;
(3) And adding the intermediate product B into a reactor filled with acetonitrile, then adding halogenated alkane, carrying out reflux reaction for 20-40 h at 75-95 ℃, carrying out reduced pressure concentration after the reaction is finished, and then carrying out separation and purification to obtain the required quaternary ammonium salt.
The further improvement is that: the molar ratio of the N, N-dimethyl allyl amine to 1,2-ethanedithiol is 1.
The further improvement is that: the photoinitiator is any one or a mixture of more than two of benzoin ethyl ether, benzophenone, 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl phenyl ketone, 2-benzyl 2-dimethylamino-1- (4-morpholinyl phenyl) butanone and isopropyl thioxanthone.
The further improvement is that: the dosage of the photoinitiator is 0.8-2.5% of the total mass of the N, N-dimethylallylamine and 1,2-ethanedithiol.
The further improvement is that: the radiation intensity of the ultraviolet light is 150-300 mW/cm2The irradiation distance is 8-14 cm, and the irradiation time is 2-6 min.
The further improvement is that: the molar ratio of the gamma-glycidyl ether propyl trimethoxy silane to the intermediate product A is 1.2-2.
The further improvement is that: the molar ratio of the intermediate product B to the halogenated alkane is 1:1-1.5.
The further improvement is that: the adhesive comprises the following raw material components in parts by weight: 40 to 60 parts of acrylic ester lauryl ester, 20 to 30 parts of acrylic acid-2-ethyl diester, 3 to 10 parts of styrene, 5 to 15 parts of acrylic acid, 0.3 to 0.8 part of dibenzoyl peroxide, 80 to 100 parts of organic solvent, 35 to 45 parts of talcum powder and 6 to 12 parts of tackifying modifier;
the tackifying modifier is prepared according to the following steps: adding (acryloxymethyl) phenyl ethyl trimethoxy silane, allyl glycidyl ether, N-dimethyl acrylamide, ethyl acetate accounting for 60-80% of the mass of an ethyl acetate solvent and azobisisobutyronitrile accounting for 15-25% of the mass of the azobisisobutyronitrile into a reaction kettle, heating to 70-80 ℃, reacting for 0.5-1 h, uniformly mixing the rest ethyl acetate and the azobisisobutyronitrile, slowly dripping into the reaction kettle, and continuously reacting for 2-4 h after dripping is finished to obtain the tackifying modifier.
The further improvement is that: the mass ratio of the (acryloyloxymethyl) phenyl ethyl trimethoxy silane to the allyl glycidyl ether to the N, N-dimethylacrylamide to the ethyl acetate to the azobisisobutyronitrile is 2-4:3-6.
By adopting the technical scheme, the invention has the beneficial effects that:
compared with the traditional production process, the glass beads have the advantages that through the electrostatic adsorption effect, plants are arranged on the surface of the PE/PET composite film, high-temperature treatment is not needed, and the follow-up stripping of the glass beads and the composite film is simpler. Specifically, the surface of the glass beads is modified by using a specially-made quaternary ammonium salt, so that the surfaces of the glass beads are positively charged, static electricity is adsorbed on the surface of the PE/PET composite membrane, electrostatic repulsion exists among the glass beads, and the bead overlapping phenomenon is not easy to occur in the bead planting process. The quaternary ammonium salt is prepared by taking N, N-dimethylallylamine and 1,2-ethanedithiol as raw materials and performing multi-step reactions including a mercapto-alkene click reaction, a ring opening reaction and a quaternization reaction, and the introduced quaternary ammonium group not only enables glass beads to have positive charges, but also enables the glass beads to have antibacterial property and inhibits the propagation of bacteria; the introduced ether bond structure improves the wear resistance and flexibility of the glass beads.
The traditional production process of the reflective fabric applies glue on the surfaces of the glass beads for multiple times, so that gaps among the glass beads are filled with the glue, the moving space is small, and the whole thickness of a glue layer is thick, so that the produced product is relatively hard and poor in flexibility. This application is not direct rubber coating on glass bead, but passes through hot rolling with the dry glue that gluing agent stoving formed and compound with nylon cloth, again with the PE PET complex film after the electroplating compound, still has the space between the glass bead like this, and the scope of activity is big under the exogenic action to make the reflection of light surface fabric of production more soft resistant book. The glue layer in the application is thinner, so that the thickness of the product can reach 9-10 threads, and the thickness of the glue layer is thicker due to repeated gluing of the reflective fabric of the traditional production process, so that the thickness of the product can only reach 14 threads. The nylon cloth is uneven due to the cloth patterns on the nylon cloth, the nylon cloth comprises a plurality of grooves, the adhesive is directly compounded with the nylon cloth, the grooves in the nylon cloth are filled with dry adhesive, the adhesion is better, and the nylon cloth is not easy to separate.
Styrene is used as a hard monomer, acrylate lauryl ester and acrylic acid-2-ethyl adipate are used as soft monomers, acrylic acid is used as a functional monomer, a proper amount of tackifying modifier and inorganic filler are added to prepare the adhesive, and the components have synergistic effect with each other, so that the comprehensive performance of the adhesive is improved. Although the traditional acrylic resin adhesive has high curing speed and low cost, the bead-grasping force of the traditional acrylic resin adhesive is deviated, and the glass beads are difficult to keep high firmness in the adhesive. Acrylic acid is utilized to react with an epoxy group of the tackifying modifier, a siloxane bond is introduced, hydrolytic condensation can be generated, the adhesion to glass beads and a metal coating is improved, and the water washing resistance of the adhesive is enhanced; the benzene ring rigid structure is introduced, so that the cohesive force of the adhesive can be enhanced, and the adhesion of the adhesive is improved; the ether bond is introduced to improve the washing resistance of the adhesive. The dimethylacrylamide contains double bonds and amide groups, and is easy to carry out polymerization reaction with other monomers under the action of an initiator, and the formed copolymer has excellent wear resistance and weather resistance. The carboxyl and the epoxy can react, but the reactivity is not high, so that the grafting cannot be completed during the grafting, and the residual part of the oligomer containing the epoxy group has small molecular weight, can be completely spread on the bonded surface (namely nylon cloth), is fully wetted and has good bonding effect on a channel. The epoxy group can also improve the adhesion force to the glass beads and the metal coating, so that the wear resistance of the reflective fabric is improved, and the probability of reduction of the reflective performance caused by easy falling of the glass beads is effectively avoided. The production cost of the acrylic resin adhesive can be greatly reduced by adding the inorganic filler talcum powder, but the quality of the acrylic resin adhesive is reduced by adding a large amount of talcum powder, so that only a small amount of talcum powder is added during the production of the traditional acrylic resin adhesive. A large amount of talcum powder is added into the raw materials of the adhesive, but the performance of the product is not greatly deteriorated, which may be the result of adjusting and optimizing the proportion of the added tackifying modifier and various monomer raw materials.
The flexibility of the reflective fabric is also influenced by the adopted adhesive, and the adhesive provided by the application is subjected to the optimized design of the formula components, so that the flexibility of the reflective fabric is obviously improved, and the effect is superior to that of a commercial acrylic resin adhesive.
Detailed Description
The following detailed description will be provided for the embodiments of the present invention with reference to specific embodiments, so that how to apply the technical means to solve the technical problems and achieve the technical effects can be fully understood and implemented.
Unless otherwise indicated, the techniques employed in the examples are conventional and well known to those skilled in the art, and the reagents and products employed are also commercially available. The source, trade name and if necessary the constituents of the reagents used are indicated at the first appearance.
Example 1
A production process of an ultra-soft reflective fabric comprises the following steps:
s1, pretreating glass beads
Dissolving quaternary ammonium salt in a solvent to prepare a quaternary ammonium salt solution with the concentration of 0.5wt%, simultaneously adjusting the pH value of the solution to be within the range of 2.5-4.5, then adding glass beads, stirring for 80min at 35 ℃, filtering, washing and drying to obtain glass beads with positive charges on the surface;
the quaternary ammonium salt is prepared by the following method:
(1) Dissolving N, N-dimethylallylamine in dimethylformamide, adding benzoin ethyl ether and 1,2-ethanedithiol, carrying out mercapto-ene click reaction by ultraviolet irradiation to obtain an intermediate product A,
the molar ratio of the N, N-dimethylallylamine to 1,2-ethanedithiol is 1.5, the dosage of benzoin ethyl ether is 0.8 percent of the total mass of the N, N-dimethylallylamine and 1,2-ethanedithiol, and the radiation intensity of the ultraviolet light is 150mW/cm2The irradiation distance of the ultraviolet lamp is 8cm, and the irradiation time is 6min;
(2) Adding gamma-glycidyl ether propyl trimethoxy silane into a reactor filled with ethanol, slowly dripping the intermediate product A into the reactor after the intermediate product A is dissolved in the ethanol, wherein the molar ratio of the gamma-glycidyl ether propyl trimethoxy silane to the intermediate product A is 1.2, and stirring and reacting for 20 hours at 25 ℃ to obtain an intermediate product B;
(3) Adding the intermediate product B into a reactor filled with acetonitrile, then adding methyl chloride, wherein the molar ratio of the intermediate product B to the methyl chloride is 1:1, carrying out reflux reaction at 75 ℃ for 40h, carrying out reduced pressure concentration after the reaction is finished, and then carrying out separation and purification to obtain the required quaternary ammonium salt;
s2, low-temperature electrostatic plant
Under the temperature condition of 30 ℃, the glass beads are used for planting plants on the surface of the PE/PET composite film through electrostatic adsorption;
s3, electroplating
Electroplating the plant PE/PET composite film to coat a metal coating on the surface of the glass microsphere to form a reflecting layer, wherein the coating is not needed before electroplating;
s4, preparation of base cloth layer
Coating a layer of adhesive on a release film, drying to form dry adhesive, and then laminating the dry adhesive with nylon cloth through a hot roller to form a base cloth layer, wherein the drying temperature and the hot roller temperature are both in the range of 60-85 ℃, the drying temperature of the embodiment is 85 ℃, and the hot roller temperature is 60 ℃;
the adhesive comprises the following raw material components in parts by weight: 40 parts of acrylate lauryl ester, 20 parts of acrylic acid-2-ethyl diester, 3 parts of styrene, 5 parts of acrylic acid, 0.3 part of dibenzoyl peroxide, 80 parts of organic solvent, 35 parts of talcum powder and 6 parts of tackifying modifier;
the tackifying modifier is prepared according to the following steps: firstly, weighing the following raw materials in parts by weight: 2 parts of (acryloxymethyl) phenylethyltrimethoxysilane, 3 parts of allyl glycidyl ether, 12 parts of N, N-dimethylacrylamide, 30 parts of ethyl acetate and 0.2 part of azobisisobutyronitrile, then adding the (acryloxymethyl) phenylethyltrimethoxysilane, the allyl glycidyl ether, the N, N-dimethylacrylamide, ethyl acetate accounting for 60 percent of the mass of an ethyl acetate solvent and azobisisobutyronitrile accounting for 15 percent of the mass of the azobisisobutyronitrile into a reaction kettle, heating to 70 ℃, reacting for 1 hour, uniformly mixing the rest of the ethyl acetate and the azobisisobutyronitrile, slowly dripping the mixture into the reaction kettle, and continuously reacting for 4 hours after dripping is finished to obtain the tackifying modifier;
s5, compounding
And (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
Example 2
A production process of an ultra-soft reflective fabric comprises the following steps:
s1, pretreating glass beads
Dissolving quaternary ammonium salt in a solvent to prepare a quaternary ammonium salt solution with the concentration of 2wt%, adjusting the pH value of the solution to be within the range of 2.5-4.5, then adding glass beads, stirring for 60min at 40 ℃, filtering, washing and drying to obtain glass beads with positive charges on the surface;
the quaternary ammonium salt is prepared by the following method:
(1) Dissolving N, N-dimethyl allyl amine in dimethyl formamide, adding 1-hydroxycyclohexyl phenyl ketone and 1,2-ethanedithiol, irradiating by ultraviolet light to generate mercapto-alkene click reaction to obtain an intermediate product A,
the molar ratio of the N, N-dimethylallylamine to 1,2-ethanedithiol is 1.8, the dosage of the 1-hydroxycyclohexyl phenyl ketone is 1.5 percent of the total mass of the N, N-dimethylallylamine and 1,2-ethanedithiol, and the radiation intensity of the ultraviolet light is 240mW/cm2The irradiation distance is 10cm, and the irradiation time is 4min;
(2) Adding gamma-glycidyl ether propyl trimethoxy silane into a reactor filled with ethanol, slowly dropwise adding an intermediate product A into the reactor after the intermediate product A is dissolved in the ethanol, wherein the molar ratio of the gamma-glycidyl ether propyl trimethoxy silane to the intermediate product A is 1.6, and stirring and reacting for 14h at 35 ℃ to obtain an intermediate product B;
(3) Adding the intermediate product B into a reactor filled with acetonitrile, then adding bromoethane, wherein the molar ratio of the intermediate product B to the bromoethane is 1.2, carrying out reflux reaction at 85 ℃ for 30h, carrying out reduced pressure concentration after the reaction is finished, and then carrying out separation and purification to obtain the required quaternary ammonium salt;
s2, low-temperature electrostatic plant
Under the temperature condition of 35 ℃, the glass beads are used for planting plants on the surface of the PE/PET composite film through electrostatic adsorption;
s3, electroplating
Electroplating the plant PE/PET composite film to coat a metal coating on the surface of the glass microsphere to form a reflecting layer, wherein the coating is not needed before electroplating;
s4, preparation of base cloth layer
Coating a layer of adhesive on a release film, drying to form dry adhesive, and then laminating the dry adhesive with nylon cloth through a hot roller to form a base cloth layer;
the adhesive comprises the following raw material components in parts by weight: 50 parts of acrylate lauryl ester, 25 parts of acrylic acid-2-ethyl diester, 6 parts of styrene, 10 parts of acrylic acid, 0.5 part of dibenzoyl peroxide, 90 parts of organic solvent, 40 parts of talcum powder and 9 parts of tackifying modifier;
the tackifying modifier is prepared according to the following steps: firstly, weighing the following raw materials in parts by weight: 3 parts of (acryloxymethyl) phenylethyl trimethoxysilane, 5 parts of allyl glycidyl ether, 16 parts of N, N-dimethylacrylamide, 35 parts of ethyl acetate and 0.3 part of azobisisobutyronitrile, then adding (acryloxymethyl) phenylethyl trimethoxysilane, allyl glycidyl ether, N-dimethylacrylamide, ethyl acetate accounting for 70% of the mass of an ethyl acetate solvent and azobisisobutyronitrile accounting for 20% of the mass of the azobisisobutyronitrile into a reaction kettle, heating to 75 ℃, reacting for 0.7h, uniformly mixing the rest of the ethyl acetate and the azobisisobutyronitrile, slowly dripping the mixture into the reaction kettle, and continuing to react for 3h after dripping is finished to obtain the tackifying modifier;
s5, compounding
And (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
Example 3
A production process of an ultra-soft reflective fabric comprises the following steps:
s1, pretreating glass beads
Dissolving quaternary ammonium salt in a solvent to prepare a quaternary ammonium salt solution with the concentration of 3wt%, adjusting the pH value of the solution to be within the range of 2.5-4.5, then adding glass beads, stirring for 40min at 50 ℃, filtering, washing and drying to obtain glass beads with positive charges on the surface;
the quaternary ammonium salt is prepared by the following method:
(1) Dissolving N, N-dimethylallylamine in dimethylformamide, adding isopropyl thioxanthone and 1,2-ethanedithiol, irradiating by ultraviolet light to generate mercapto-ene click reaction to obtain an intermediate product A,
the molar ratio of the N, N-dimethylallylamine to 1,2-ethanedithiol is 1:1, the dosage of the isopropyl thioxanthone is 2.5 percent of the total mass of the N, N-dimethylallylamine and 1,2-ethanedithiol, and the radiation intensity of the ultraviolet light is 300mW/cm2The irradiation distance is 14cm, and the irradiation time is 2min;
(2) Adding gamma-glycidyl ether propyl trimethoxy silane into a reactor filled with ethanol, slowly dripping the intermediate product A into the reactor after the intermediate product A is dissolved in the ethanol, wherein the molar ratio of the gamma-glycidyl ether propyl trimethoxy silane to the intermediate product A is 1:2, and stirring and reacting for 8 hours at 45 ℃ to obtain an intermediate product B;
(3) Adding the intermediate product B into a reactor filled with acetonitrile, then adding bromoethane, wherein the molar ratio of the intermediate product B to the bromoethane is 1.5, carrying out reflux reaction at 95 ℃ for 20 hours, carrying out reduced pressure concentration after the reaction is finished, and then carrying out separation and purification to obtain the required quaternary ammonium salt;
s2, low-temperature electrostatic plant
Under the temperature condition of 40 ℃, the glass beads are planted on the surface of the PE/PET composite film through electrostatic adsorption;
s3, electroplating
Electroplating the plant PE/PET composite film to coat a metal coating on the surface of the glass microsphere to form a reflecting layer, wherein the coating is not needed before electroplating;
s4, preparation of base fabric layer
Coating a layer of adhesive on the release film, drying to form dry adhesive, and then pressing the dry adhesive with nylon cloth through a hot roller to form a base cloth layer;
the adhesive comprises the following raw material components in parts by weight: 60 parts of acrylic ester lauryl ester, 30 parts of acrylic acid-2-ethyl diester, 10 parts of styrene, 15 parts of acrylic acid, 0.8 part of dibenzoyl peroxide, 100 parts of organic solvent, 45 parts of talcum powder and 12 parts of tackifying modifier;
the tackifying modifier is prepared according to the following steps: firstly, weighing the following raw materials in parts by weight: 4 parts of (acryloxymethyl) phenylethyl trimethoxysilane, 6 parts of allyl glycidyl ether, 20 parts of N, N-dimethylacrylamide, 40 parts of ethyl acetate and 0.4 part of azobisisobutyronitrile, then adding (acryloxymethyl) phenylethyl trimethoxysilane, allyl glycidyl ether, N-dimethylacrylamide, ethyl acetate accounting for 80% of the mass of an ethyl acetate solvent and azobisisobutyronitrile accounting for 25% of the mass of the azobisisobutyronitrile into a reaction kettle, heating to 80 ℃, reacting for 0.5h, uniformly mixing the rest of the ethyl acetate and the azobisisobutyronitrile, slowly dripping the mixture into the reaction kettle, and continuing to react for 2h after dripping is finished to obtain the tackifying modifier;
s5, compounding
And (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
Comparative example 1
The production process of the reflective fabric is different from that of the embodiment 1 in that: the adhesive adopted in S4 is the existing adhesive, and the specific formula is disclosed in patent No. CN201410069828.2.
Comparative example 2
The production process of the reflective fabric is different from that of the embodiment 1 in that: by adopting the traditional process, glass microsphere high-temperature plants are arranged on the surface of the PE/PET composite membrane.
Comparative example 3
The production process of the reflective fabric is different from that of the comparative example 2 in that: the adopted adhesive is the conventional adhesive, and the specific formula is disclosed in patent No. CN201410069828.2.
Comparative example 4
The production process of the reflective fabric is different from that of the embodiment 1 in that: the adhesive comprises 5 parts of talcum powder.
Comparative example 5
The production process of the reflective fabric is different from that of the embodiment 1 in that: the adhesive formula refers to patent number CN201410069828.2, and 5 parts by weight of talcum powder is added.
Performance test of reflective fabric
The samples of the reflective fabrics prepared in examples 1 to 3 and the respective proportions were tested for flexibility, abrasion resistance, and wash resistance, and the results are shown in tables 1 to 2.
The softness is comprehensively judged according to the stretching linearity and the bending rigidity, wherein the stretching linearity represents the stretching difficulty of the reflective fabric sample, the smaller the numerical value is, the larger the stretching initial deformation of the reflective fabric is, the softer the hand feeling is, and the more comfortable the wearing is. In the bending characteristic test, the bending rigidity of the reflective fabric sample is tested, the bending rigidity represents the rigidity and flexibility of the reflective fabric sample, and the smaller the bending rigidity is, the softer the reflective fabric sample is. The specific test method for flexibility is as follows: cutting a reflective fabric sample into sizes of 20cm multiplied by 20cm, and testing the tensile linearity and the bending rigidity of the reflective fabric sample by adopting a pure bending tester of a fabric style evaluation system.
The wear resistance test method of the reflective fabric comprises the following steps: placing the reflective fabric sample under a microscope, and calculating the unit area (mm)2) Number of initial glass beads of the surface. Then, a Y522N type disc type fabric wear-resisting instrument is adopted, a pressurizing weight 250g and a grinding wheel A150 are selected, the glass bead surface of the reflective fabric sample is rubbed for 200 circles, and the unit area (mm) is calculated again2) And taking the number of the residual glass beads on the surface as the percentage of the number of the residual glass beads in the initial number of the glass beads as the basis for judging the wear resistance.
TABLE 1
As can be seen from table 1, compared with comparative examples 1 to 5, the reflective fabrics prepared in examples 1 to 3 of the present invention have lower tensile linearity and bending stiffness, which indicates that the reflective fabrics prepared in the present invention have better flexibility; the percentage of the number of the residual glass beads to the initial number of the glass beads after the friction is still kept above 95.7%, which shows that the adhesive has strong bead-grasping force and good adhesion to the glass beads, and can ensure that the glass beads are firmly fixed in the adhesive, so that the wear resistance of the reflective fabric is improved, and the probability of reduction of the reflective performance caused by easy falling of the glass beads is effectively avoided.
TABLE 2
As can be seen from Table 2, the reflective fabrics prepared in the embodiments 1-3 of the present invention have excellent water resistance and good reflective performance after repeated washing.
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.
Claims (10)
1. A production process of an ultra-soft reflective fabric is characterized by comprising the following steps: the method comprises the following steps:
s1, pretreating glass beads
Dissolving quaternary ammonium salt in a solvent to prepare a quaternary ammonium salt solution with the concentration of 0.5-3 wt%, adjusting the pH value of the solution to be within the range of 2.5-4.5, then adding glass beads, stirring for 40-80 min at 35-50 ℃, filtering, washing and drying to obtain glass beads with positive charges on the surface;
s2, low-temperature electrostatic plant
Under the temperature condition of 30-40 ℃, the glass beads are used for planting plants on the surface of the PE/PET composite film through electrostatic adsorption;
s3, electroplating
Electroplating the plant PE/PET composite film to coat a metal coating on the surface of the glass microsphere to form a reflecting layer, wherein the coating is not needed before electroplating;
s4, preparation of base cloth layer
Coating a layer of adhesive on a release film, drying to form dry adhesive, and then laminating the dry adhesive with nylon cloth through a hot roller to form a base cloth layer;
s5, compounding
And (3) compounding the electroplated PE/PET composite film with nylon cloth with dry glue on the surface, and stripping the PE/PET composite film to obtain the super-soft light-reflecting fabric.
2. The production process of the super-soft reflective fabric according to claim 1, characterized in that: the quaternary ammonium salt is prepared by the following method:
(1) Dissolving N, N-dimethylallylamine in dimethylformamide, adding a photoinitiator and 1,2-ethanedithiol, and irradiating by ultraviolet light to generate a mercapto-alkene click reaction to obtain an intermediate product A;
(2) Adding gamma-glycidyl ether propyl trimethoxy silane into a reactor filled with ethanol, dissolving the intermediate product A in the ethanol, slowly dripping the dissolved intermediate product A into the reactor, and stirring and reacting at 25-45 ℃ for 8-20 h to obtain an intermediate product B;
(3) And adding the intermediate product B into a reactor filled with acetonitrile, then adding halogenated alkane, carrying out reflux reaction for 20-40 h at 75-95 ℃, carrying out reduced pressure concentration after the reaction is finished, and then carrying out separation and purification to obtain the required quaternary ammonium salt.
3. The production process of the super-soft reflective fabric according to claim 2, characterized in that: the molar ratio of the N, N-dimethyl allyl amine to 1,2-ethanedithiol is 1.
4. The production process of the super-soft light-reflecting fabric according to claim 2, characterized in that: the photoinitiator is any one or a mixture of more than two of benzoin ethyl ether, benzophenone, 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl phenyl ketone, 2-benzyl 2-dimethylamino-1- (4-morpholinyl phenyl) butanone and isopropyl thioxanthone.
5. The production process of the super-soft reflective fabric according to claim 2, characterized in that: the dosage of the photoinitiator is 0.8-2.5% of the total mass of the N, N-dimethylallylamine and 1,2-ethanedithiol.
6. The production process of the super-soft light-reflecting fabric according to claim 2, characterized in that: the radiation intensity of the ultraviolet light is 150-300 mW/cm2The irradiation distance is 8-14 cm, and the irradiation time is 2-6 min.
7. The production process of the super-soft light-reflecting fabric according to claim 2, characterized in that: the molar ratio of the gamma-glycidyl ether propyl trimethoxy silane to the intermediate product A is 1.2-2.
8. The production process of the super-soft reflective fabric according to claim 2, characterized in that: the molar ratio of the intermediate product B to the halogenated alkane is 1:1-1.5.
9. The production process of the super-soft reflective fabric according to claim 1, characterized in that: the adhesive comprises the following raw material components in parts by weight: 40 to 60 portions of acrylic ester lauryl ester, 20 to 30 portions of acrylic acid-2-ethyl diester, 3 to 10 portions of styrene, 5 to 15 portions of acrylic acid, 0.3 to 0.8 portion of dibenzoyl peroxide, 80 to 100 portions of organic solvent, 35 to 45 portions of talcum powder and 6 to 12 portions of tackifying modifier;
the tackifying modifier is prepared according to the following steps: adding (acryloxymethyl) phenyl ethyl trimethoxy silane, allyl glycidyl ether, N-dimethyl acrylamide, ethyl acetate accounting for 60-80% of the mass of an ethyl acetate solvent and azobisisobutyronitrile accounting for 15-25% of the mass of the azobisisobutyronitrile into a reaction kettle, heating to 70-80 ℃, reacting for 0.5-1 h, uniformly mixing the rest ethyl acetate and the azobisisobutyronitrile, slowly dripping into the reaction kettle, and continuously reacting for 2-4 h after dripping is finished to obtain the tackifying modifier.
10. The process for producing the super-soft light-reflecting fabric according to claim 9, wherein the process comprises the following steps: the mass ratio of the (acryloyloxymethyl) phenyl ethyl trimethoxy silane to the allyl glycidyl ether to the N, N-dimethylacrylamide to the ethyl acetate to the azobisisobutyronitrile is 2-4:3-6.
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| CN112099120A (en) * | 2020-09-15 | 2020-12-18 | 浙江夜光明光电科技股份有限公司 | Super-soft reflective cloth and preparation method thereof |
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