Manufacturing process of reflective material and composite system thereof
By using moisture-cured polyurethane resin and hot melt coating technology, combined with humidified gas curing technology, the problem of high energy consumption in traditional reflective materials is solved, and efficient and low-cost reflective materials are achieved.
Patent Information
- Application Number
- CN202510171094.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-17
- Publication Date
- 2025-05-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The production process of traditional reflective materials requires a large amount of energy, and has high production efficiency and cost.
Moisture-cured polyurethane resin is used as the adhesive, and it is coated on the glass microbead layer of the reflective bead planting film through hot melt coating technology, and is combined with the substrate to gradually cure through a humidified environment, avoiding the oven heating process.
It realizes the production of reflective materials without oven heating, saves energy, improves production efficiency and reduces costs, and is in line with the national energy-saving and consumption reduction policy.
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Figure CN119937073A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of reflective materials, and in particular to a manufacturing process of reflective materials and a composite system thereof. Background Art
[0002] In the traditional method of making reflective materials, solvent-based resin or water-based resin is directly or indirectly coated on the surface of the reflective beaded film, and then the organic solvent is evaporated or the water is evaporated by drying in an oven, and then the substrate is cold-laminated or heated-laminated in a composite manner to form the reflective material.
[0003] It can be seen that the traditional reflective material processing technology uses oven heating and curing, and whether it is electric heating or thermal oil or steam heating, it consumes a lot of energy.
[0004] Based on the above problems, the traditional reflective material manufacturing process still needs to be improved. Summary of the invention
[0005] In order to solve the above technical problems, the present application provides a process for manufacturing a reflective material, including the following manufacturing steps: Q1: Provide reflective implant film with glass beads layer, unwinding; Q2: providing a moisture-curable polyurethane resin, and applying the moisture-curable polyurethane resin to the glass microbead layer of the reflective bead-embedded film in a hot-melt manner; Q3: Providing a substrate, and compounding the moisture-curable polyurethane resin with the glass microsphere layer to form a composite material; Q4: Add humidification to gradually cure the composite material in a humidity environment of 50% to 80%, and then cure it at room temperature after rolling up to obtain a reflective material.
[0006] The present application provides a production process for the above-mentioned reflective material. The production process does not require the use of an oven heating method to produce the reflective material, which not only meets the washability requirements of the reflective material, but also saves energy. At the same time, it has higher production efficiency and lower cost, which is in line with the current national policy of energy conservation and consumption reduction.
[0007] The reflective material finally prepared in the present application includes a reflective bead-embedded film, a moisture-curable polyurethane resin layer (i.e., an adhesive layer), and a substrate connected in sequence. A glass microbead layer connected to the adhesive layer is provided on the surface of the reflective bead-embedded film.
[0008] The application of the moisture-curable polyurethane resin as an adhesive in the reflective material of the present application not only has excellent water wash resistance but also has high bonding strength. Therefore, the reflective material of the present application uses the moisture-curable polyurethane resin as an adhesive and does not need to be cured by oven heating, but is cured by humidification.
[0009] Optionally, the moisture-curable polyurethane resin comprises the following components in parts by weight: 60-65 parts of polyester polyol; Polyether polyol 5-20 parts; MDI 6-8 parts; IPDI 4-6 parts; 6-20 parts of tackifying resin; 0.2 parts of catalyst; Reactive plasticizer 4~16 parts; The preparation steps of the moisture-curable polyurethane resin are as follows: S100: preparing the polyester polyol; S200: mixing the polyester polyol and the polyether polyol and performing vacuum dehydration; S300: adding the reactive plasticizer, MDI and IPDI and mixing them evenly to form a premixed system, wherein the NCO% content in the premixed system reaches 1.8% to 2.9%; S400: The premixed system is placed in a nitrogen environment and heated to 70° C. to 90° C. for full reaction; S500: adding the remaining components into the premixed system, heating to 90° C. to 110° C., evacuating until no bubbles are generated, and discharging the material to obtain the moisture-curable polyurethane resin.
[0010] The moisture-curable polyurethane resin of the present application is produced by reacting polyester polyols and polyether polyols with isocyanates (MDI, IPDI) to produce a polyurethane prepolymer with -NCO end-capping. The isocyanate groups in the system can react with external substances containing active hydroxyl groups, such as water, to produce polyurethane groups or polyureas, thereby being cured to achieve an efficient bonding effect.
[0011] Optionally, the moisture-curable polyurethane resin further includes an antioxidant, and the antioxidant includes the following components in parts by weight: 0.1 part of 3-(3,5-di-tert-butyl-4-carboxyphenyl) propionate; γ-Glycidyloxypropyltrimethoxysilane 0.1 parts.
[0012] Optionally, the catalyst is potassium isooctanoate.
[0013] Optionally, the polyester polyol has a molecular weight of 4000-8000, a hydroxyl value of 45-50 mgKOH / g, and an acid value of 0.78-0.92 mgKOH / g.
[0014] Optionally, the polyester polyol comprises the following components in parts by weight: 12-16 parts of terephthalic acid; Isophthalic acid 5.6-8.4 parts; Sebacic acid 6.7-8.2 parts Adipic acid 5.9-7.6 parts; Ethylene glycol 10.4-13.6 parts 9.6-11.5 parts of dedeoxycholic acid; The step S100 also includes the following: S101: Add all components into a reactor to melt, introduce nitrogen, heat to 160°C~180°C, and react fully; S102: distilling out the water generated in the reactor; S103: raising the temperature to 170° C. to 230° C., adjusting the vacuum degree in the reactor to 500 Pa, and evaporating the unreacted components, side reactions and water to obtain the polyester polyol.
[0015] In step S101, each component undergoes esterification and polycondensation reaction in a reactor to generate water, and after the water is removed in step S102, a low molecular weight polyester mixture (such as low molecular weight polyester polyol) is generated in the reactor. In step S103, the excess diol and a small amount of side reaction products (such as low molecular weight polyester, aldehyde and ketone) are finally evaporated together with the residual water generated by the reaction.
[0016] Optionally, in step Q1, the moisture-curable polyurethane resin is a polyurethane prepolymer with -NCO end-capping generated by reacting polyester and / or polyether polyol with isocyanate.
[0017] Optionally, in step Q2, the reflective bead-embedded film is unrolled by an unwinding system.
[0018] Optionally, in step Q3, the moisture-curable polyurethane resin is hot-melt coated using a hot-melt coating device.
[0019] The present application also provides a composite system for implementing the above-mentioned manufacturing process, comprising: A first unwinding mechanism, used for unwinding the reflective bead-embedded film; A second unwinding mechanism, used for unwinding the substrate; A hot melt coating device, connected to the first unwinding mechanism, comprises a vacuum hot melt adhesive melter, a vacuum conveying pipe and a hot melt coating head, for melting and conveying the moisture-curing polyurethane resin and hot-melt coating the moisture-curing polyurethane resin on the reflective bead-embedded film; A pressing device, used for cold pressing or hot pressing the composite material; The humidification curing mechanism provides an environment with a humidity of 50% to 80% for curing moisture-curing polyurethane resin.
[0020] Optionally, the moisture-curable polyurethane resin is coated on the glass microbead layer by the hot melt coating head.
[0021] Optionally, during the hot melt coating process, the hot melt adhesive of the vacuum hot melt adhesive machine is frequency-controlled at 30 Hz-50 Hz, and the hot melt coating head is heated to 130° C.-180° C.
[0022] Optionally, the hot melt coating amount of the moisture-curable polyurethane resin is 20-120 g / m2.
[0023] Optionally, the glass beads of the reflective bead-embedded film have a particle size range of 45 μm-90 μm.
[0024] Optionally, the reflective bead-embedded film coated with the moisture-curable polyurethane resin and the substrate are cold-bonded or hot-bonded by a composite device.
[0025] Optionally, the composite device further comprises a heatable mold temperature unit, and the mold temperature unit is a double-roller or three-roller pressing device that uses air pressure to control the up and down movement.
[0026] Optionally, the pressing device includes: The upper roller is a heatable steel roller; The lower roller is a single roller or a double roller made of nitrile rubber.
[0027] Optionally, in step Q4, the compounding temperature is 50° C.-150° C., and the compounding pressure is controlled at 0.3 MPa-0.7 MPa.
[0028] Optionally, the substrate is fabric, hot melt adhesive or leather.
[0029] Optionally, the substrate is TC cloth, chemical fiber cloth, or flame-retardant cloth containing a polyurethane coating.
[0030] Optionally, the composite material is maintained in an environment of a temperature of 23-28° C. and a humidity of 50% for 48-96 hours.
[0031] The moisture-curable polyurethane resin of the present application is cured by contact with moisture, and does not need to be cured in an oven, and can be used as an adhesive for reflective materials, meeting the requirements of reflective materials being resistant to washing. In addition, the reflective material finally prepared by the moisture-curable polyurethane resin of the present application has a simple process and does not need to go through an oven drying process, which not only saves energy consumption, but also has higher production efficiency and lower costs, which is in line with the current national energy-saving and consumption-reducing policies. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 A flow chart of the manufacturing process of the reflective material of the present application; Figure 2 This is a schematic diagram of the structure of the reflective material of this application.
[0033] The reference numerals in the figures are described as follows: 1. Reflective bead film; 11. Glass bead layer; 2. Adhesive layer; 3. Base material. DETAILED DESCRIPTION
[0034] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
[0035] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application.
[0036] An embodiment of the present application provides a reflective material, including a reflective bead-embedded film, an adhesive layer, and a substrate connected in sequence. A glass bead layer connected to the adhesive layer is provided on the surface of the reflective bead-embedded film, and the adhesive layer is a moisture-curable polyurethane resin that is resistant to washing.
[0037] The present application also provides a manufacturing process of the above-mentioned reflective material, including the following manufacturing steps: Q1: Provide reflective implant film with glass beads layer, unwinding; Q2: Provide moisture-curable polyurethane resin, and apply the moisture-curable polyurethane resin to the glass microbead layer of the reflective bead-embedded film in a hot-melt manner; Q3: Provide a substrate and compound it with a glass bead layer through a moisture-curable polyurethane resin to form a composite material; Q4: Add humidification to make the composite material gradually solidify in a humidity environment of 50% to 80%, and then solidify at room temperature after rolling up to obtain the reflective material.
[0038] The manufacturing process of the above-mentioned reflective material mainly includes a reflective bead film unwinding process, a hot melt coating process of a moisture-curable polyurethane resin, a compounding process, and a humidification curing process. In step Q1, the moisture-curable polyurethane resin is a polyurethane prepolymer with -NCO end-capping generated by the reaction of polyester and / or polyether polyol with isocyanate.
[0039] In step Q2, the reflective bead-embedded film is unrolled by an unwinding system.
[0040] In step Q3, the moisture-curable polyurethane resin is hot-melt coated using a hot-melt coating device.
[0041] The present application discloses a production method that is more environmentally friendly and more efficient. In the production process, there is no need to use an oven to heat the volatile solvent or water to directly compound the reflective material. The present application adopts a hot melt coating method, and directly compounds the substrate to form a reflective material after coating with a moisture-curing special polyurethane resin. The traditional reflective material processing technology uses oven drying and heating. Whether it is electric heating or thermal oil or steam heating, it consumes a lot of energy. The new processing technology disclosed in the present application does not need to use oven heating to produce reflective materials, which saves a lot of energy during the production process. At the same time, the production efficiency is higher and the cost is lower, which complies with the current national energy-saving and consumption-reducing policies.
[0042] Preferably, the moisture-curable polyurethane resin comprises the following components in parts by weight: 60-65 parts of polyester polyol; Polyether polyol 5-20 parts; MDI 6-8 parts; IPDI 4-6 parts; 6-20 parts of tackifying resin; 0.2 parts of catalyst; The preparation steps of moisture curing polyurethane resin are as follows: S100: preparation of polyester polyol; S200: Mixing polyester polyol and polyether polyol and performing vacuum dehydration; S300: Add reactive plasticizer, MDI and IPDI and mix evenly to form a premixed system; S400: The premixed system is placed in a nitrogen environment and heated to 70°C~90°C for full reaction; S500: Add the remaining components into the premixed system, heat to 90°C~110°C, evacuate until no bubbles are generated, and discharge the material to obtain moisture-curing polyurethane resin.
[0043] Among them, in step S400, after the reaction is completed, the NCO% content in the premixed system reaches 1.8%~2.9%.
[0044] The moisture-curable polyurethane resin also includes an antioxidant, which includes the following components in parts by weight: 0.1 part of 3-(3,5-di-tert-butyl-4-carboxyphenyl) propionate; γ-Glycidyloxypropyltrimethoxysilane 0.1 parts.
[0045] The moisture-curable polyurethane resin further includes 4 to 16 parts by weight of a reactive plasticizer.
[0046] In some embodiments, more specifically, the steps for preparing the moisture-curable polyurethane resin are as follows: Preparation of polyester polyols; Add 5-20 parts by weight of polyether polyol and 60-65 parts by weight of polyester polyol into a reaction device, vacuum dehydrate, and then cool to 80°C; While stirring the reaction device, add 4-16 parts by weight of reactive plasticizer and 6-8 parts by weight of MDI, and then add 4-6 parts of IPDI to form a premixed system; Then the temperature of the reaction device is raised to 70-90°C, nitrogen is filled for protection, and the reaction is carried out for 2-3 hours. After the reaction is completed, a sample is taken out from the reaction device to detect the NCO% content, and the NCO% content of the premixed system is controlled at 1.8%-2.9%, and the next step is continued; Then add 6-20 parts by weight of tackifying resin and 0.2 parts by weight of catalyst, heat the reaction device to 90-110° C., evacuate until no bubbles appear, discharge the material, and seal and package to obtain moisture-curable polyurethane resin.
[0047] Preferably, the catalyst may be potassium isooctanoate, and the tackifying resin may be C9 petroleum resin.
[0048] In some embodiments, in the raw materials for preparing the moisture-curable polyurethane resin, the polyether polyol has a molecular weight of 4000-8000, a hydroxyl value of 45-50 mgKOH / g, an acid value of 0.78-0.92 mgKOH / g, and has good hydrolysis resistance and excellent acid and alkali resistance.
[0049] Preferably, the polyester polyol comprises the following components in parts by weight: 12-16 parts of terephthalic acid; Isophthalic acid 5.6-8.4 parts; Sebacic acid 6.7-8.2 parts Adipic acid 5.9-7.6 parts; Ethylene glycol 10.4-13.6 parts 9.6-11.5 parts of dedeoxycholic acid; The above step S100, the step of preparing polyester polyol, further comprises the following specific steps: S101: adding all the above components into a reactor to melt, introducing nitrogen, heating to 160°C-180°C, and fully reacting; S102: Distilling out the water generated in the reactor; S103: Raise the temperature to 170°C~230°C, adjust the vacuum degree in the reactor to 500Pa, evaporate the unreacted components, side reactions and water, and obtain polyester polyol.
[0050] Among them, in step S101, each component undergoes esterification and polycondensation reaction in the reactor to generate water, and after the water is removed in step S102, a low-molecular-weight polyester mixture (such as low molecular weight polyester polyol) is generated in the reactor.
[0051] In step S103, the excess diol and a small amount of side reaction products (such as low molecular weight polyester, aldehyde and ketone) are finally evaporated together with the residual water generated by the reaction.
[0052] More specifically, the preparation process of polyester polyol is as follows: First, 12-16 parts by weight of terephthalic acid, 5.6-8.4 parts by weight of isophthalic acid, 6.7-8.2 parts by weight of sebacic acid, 5.9-7.6 parts by weight of adipic acid, 10.4-13.6 parts by weight of ethyl alcohol, and 9.6-11.5 parts by weight of sebacic acid are added into a reactor to be melted, nitrogen is introduced, and the reactor is heated to 160° C. to 180° C. for esterification and polycondensation reaction to generate water, and the reaction is fully reacted; The water produced in the reactor is gradually evaporated, and a low-molecular-weight polyester mixture (such as low molecular weight polyester polyol) is generated in the reactor; As the water evaporates, the temperature in the reactor gradually increases. When the temperature rises to 170-230°C, the vacuum degree drops to about 500 Pa. Finally, the excess diol and a small amount of side reaction products (such as low molecular weight polyesters, aldehydes and ketones) are evaporated together with the residual water generated by the reaction to obtain polyester polyols.
[0053] The present application also provides a process for manufacturing a reflective material, wherein the above-mentioned moisture-cured polyurethane resin is used as an adhesive for the reflective material.
[0054] refer to Figure 1 to Figure 2 The reflective material produced in this application mainly includes three layers: a reflective bead-embedded film 1, an adhesive layer 2 (i.e., moisture-cured polyurethane resin), and a substrate 3. The surface of the reflective bead-embedded film 1 is a glass microbead layer 11, and the moisture-cured polyurethane resin 2 is located between the reflective bead-embedded film and the substrate and is used to bond the two.
[0055] In some embodiments, the hot melt coating device includes a vacuum hot melt adhesive melter, a vacuum delivery pipe, and a hot melt coating head. During the hot melt coating process, the hot melt adhesive of the vacuum hot melt adhesive melter is frequency-controlled at 30 Hz-50 Hz, and the hot melt coating head is heated to 130°C-180°C.
[0056] The hot melt coating amount of the moisture-curable polyurethane resin is 20-120 g / m2, preferably 75-85 g / m2.
[0057] The particle size of the glass beads of the reflective implanted bead film ranges from 45μm to 110μm, and the preferred particle size of the glass beads is 53μm to 90μm. In step Q4, the substrate is unwound by the unwinding system. The reflective beaded film and the substrate are cold-bonded or hot-bonded by the laminating device. The laminating temperature is 50°C-150°C, the laminating pressure is controlled at 0.3MPa-0.7MPa, and the optimal laminating pressure is set at 0.5MPa-0.6MPa.
[0058] The substrate is various textile fabrics or various hot melt adhesives or various types of leather bases, preferably TC cloth, chemical fiber cloth, and flame retardant cloth containing polyurethane coating.
[0059] In step Q5, the composite material is maintained at a temperature of 23-28° C. and a humidity of 50% for 48-96 hours; and is rolled up by a rolling system.
[0060] In some embodiments, in order to ensure the uniformity of coating, the hot melt coating head adopts a dual-channel design, the coating amount is controlled at 25 g / m2~150 g / m2, and the coating amount accuracy is controlled at ±3 g / m2; the temperature of the hot melt coating head is controllable and the temperature control range is 100°C~260°C, and the temperature control accuracy is ±2°C.
[0061] The vacuum conveying pipe is a high temperature resistant vacuum conveying pipe, which can withstand a pressure range of 5-150MPa and a temperature range of 80℃~380℃. The inner tube of the vacuum conveying pipe is made of Teflon. In order to ensure the demand for high-speed coating, the inner tube diameter is not less than 40mm. A flow control valve is installed at the hot melt coating head to control the flow in the conveying pipe.
[0062] The vacuum hot melt glue machine adopts a melting cylinder type glue melting method, the glue melting efficiency is not less than 240Kg / h, the temperature control range is 120℃-280℃, and the suitable resin viscosity range is 0~10000cps. The glue melting efficiency and glue output speed are controlled by frequency conversion and are controlled at 30hz-50hz, which can be adjusted according to the changes in coating amount and coating vehicle speed.
[0063] Examples 1 to 3 are preparation examples of polyester polyols, Examples 4 to 6 are preparation examples of moisture-curable polyurethane resins, and Example 7 is a preparation example of reflective materials. Example
[0064] The polyester polyol comprises the following components in parts by weight: 12 parts of terephthalic acid; Isophthalic acid 5.6 parts; 6.7 parts of sebacic acid Adipic acid 5.9 parts; 10.4 parts of ethylene glycol 9.6 parts of dedeoxycholic acid; The preparation of the polyester polyol in step S100 further comprises the following steps: S101: Add all components into a reactor to melt, introduce nitrogen, heat to 160°C, and react fully; S102: Distilling out the water generated in the reactor; S103: The temperature is raised to 170° C., and the vacuum degree in the reactor is adjusted to 500 Pa to evaporate the unreacted components, side reactions and water, thereby obtaining polyester polyol.
[0065] Example 2 The polyester polyol comprises the following components in parts by weight: 14 parts of terephthalic acid; 7 parts of isophthalic acid; 7.5 parts of sebacic acid Adipic acid 6.5 parts; 12 parts of ethylene glycol 11 parts of dedeoxycholic acid; The preparation of the polyester polyol in step S100 further comprises the following steps: S101: Add all components into a reactor to melt, introduce nitrogen, heat to 170°C, and react fully; S102: Distilling out the water generated in the reactor; S103: The temperature is raised to 200° C., and the vacuum degree in the reactor is adjusted to 500 Pa, and unreacted components, side reactions and water are evaporated to obtain polyester polyol.
[0066] Example 3 The polyester polyol comprises the following components in parts by weight: 16 parts of terephthalic acid; 8.4 parts of isophthalic acid; 8.2 parts of sebacic acid Adipic acid 7.6 parts; Ethylene glycol 13.6 parts 11.5 parts of dedeoxycholic acid; The preparation of the polyester polyol in step S100 further comprises the following steps: S101: Add all components into a reactor to melt, introduce nitrogen, heat to 180°C, and react fully; S102: Distilling out the water generated in the reactor; S103: The temperature is raised to 230° C., and the vacuum degree in the reactor is adjusted to 500 Pa to evaporate the unreacted components, side reactions and water, thereby obtaining polyester polyol.
[0067] Example 4 The moisture-curable polyurethane resin comprises the following components in parts by weight: 60 parts of polyester polyol; 5 parts of polyether polyol; MDI 6 parts; IPDI 4 parts; 6 parts of tackifying resin; 0.2 parts of catalyst; The preparation steps of moisture-curing polyurethane resin are as follows: S100: preparation of polyester polyol; S200: Mixing polyester polyol and polyether polyol and performing vacuum dehydration; S300: Add MDI and IPDI and mix evenly to form a premixed system; S400: The premixed system is placed in a nitrogen environment and heated to 70°C for full reaction; S500: Add tackifying resin and catalyst into the premixed system, heat to 90°C, evacuate until no bubbles are generated, and discharge the material to obtain moisture-curing polyurethane resin.
[0068] Example 5 The moisture-curable polyurethane resin comprises the following components in parts by weight: 62 parts of polyester polyol; 18 parts of polyether polyol; MDI 7 parts; IPDI 5 copies; 13 parts of tackifying resin; 0.2 parts of catalyst; The preparation steps of moisture-curing polyurethane resin are as follows: S100: preparation of polyester polyol; S200: Mixing polyester polyol and polyether polyol and performing vacuum dehydration; S300: Add MDI and IPDI and mix evenly to form a premixed system; S400: The premixed system is placed in a nitrogen environment and heated to 80°C for full reaction; S500: Add tackifying resin and catalyst into the premixed system, heat to 100°C, evacuate until no bubbles are generated, and discharge the material to obtain moisture-curing polyurethane resin.
[0069] Example 6 The moisture-curable polyurethane resin comprises the following components in parts by weight: 65 parts of polyester polyol; 20 parts of polyether polyol; MDI 8 parts; IPDI 6 parts; 20 parts of tackifying resin; 0.2 parts of catalyst; The preparation steps of moisture-curing polyurethane resin are as follows: S100: preparation of polyester polyol; S200: Mixing polyester polyol and polyether polyol and performing vacuum dehydration; S300: Add MDI and IPDI and mix evenly to form a premixed system; S400: The premixed system is placed in a nitrogen environment and heated to 90°C for full reaction; S500: Add tackifying resin and catalyst into the premixed system, heat to 110°C, evacuate until no bubbles are generated, and discharge the material to obtain moisture-curing polyurethane resin.
[0070] Example 7 A process for producing a reflective material includes the following steps: Q1: Take the moisture-curable polyurethane resin prepared in Examples 4 to 6; Q2: Provide reflective beaded film and unwind; Q3: Apply moisture-curing polyurethane resin to the glass bead layer of the reflective bead film by hot melt; Q4: Provide a substrate and compound it with a glass bead layer through a moisture-curing polyurethane resin; Q5: Add humidification to make the composite material gradually solidify in a humidity environment of 70%~80%. After rolling up, solidify it at room temperature for 48 hours to obtain the reflective material.
[0071] Performance Testing The moisture-curable polyurethane resin prepared in Examples 4-6 was used to prepare reflective material samples 1-3 in accordance with steps Q1-Q5. Three reflective products on the market, 3M9910, D6610, and YSL205, were used as comparative examples to conduct three performance tests on home washing performance, industrial washing performance, and dry cleaning performance. The test method is as follows: 1. Home washing performance test: Test the samples according to the washing method specified in ISO6330:6N, and obtain the retroreflection coefficient value of the samples after 100 washing cycles; Evaluation criteria: The larger the retroreflection coefficient value of the sample in the test, the better the washing resistance.
[0072] 2. Industrial washing performance test: Test the samples according to the industrial washing method specified in ISO15797, and obtain the retroreflection coefficient of the samples after 30 washing cycles; Evaluation criteria: The larger the retroreflection coefficient value of the sample in the test, the better the washing resistance.
[0073] Dry cleaning performance test: Test the sample according to the dry cleaning method specified in ISO3175, and obtain the retroreflection coefficient of the sample after 30 dry cleaning cycles; Evaluation criteria: The larger the retroreflection coefficient value of the sample in the test, the better the washing resistance.
[0074] The performance parameters of the final products obtained in each embodiment of the present application and the comparative examples are shown in Table 1: Table 1 The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification. When the technical features in different embodiments are embodied in the same figure, it can be regarded that the figure also discloses the combination examples of the various embodiments involved.
[0075] The above-mentioned embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the patent application. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application.
Claims
1. The manufacturing process of the reflective material is characterized by: The production steps include: Q1: Provide reflective implant film with glass beads layer, unwinding; Q2: providing a moisture-curable polyurethane resin, and applying the moisture-curable polyurethane resin to the glass microbead layer of the reflective bead-embedded film in a hot-melt manner; Q3: Providing a substrate, and compounding the moisture-curable polyurethane resin with the glass microsphere layer to form a composite material; Q4: Add humidification to gradually cure the composite material in a humidity environment of 50% to 80%, and then cure it at room temperature after rolling up to obtain a reflective material.
2. The manufacturing process according to claim 1, characterized in that: The moisture-curable polyurethane resin comprises the following components in parts by weight: 60-65 parts of polyester polyol; Polyether polyol 5-20 parts; MDI 6-8 parts; IPDI 4-6 parts; 6-20 parts of tackifying resin; 0.2 parts of catalyst; Reactive plasticizer 4~16 parts; The preparation steps of the moisture-curable polyurethane resin are as follows: S100: preparing the polyester polyol; S200: mixing the polyester polyol and the polyether polyol and performing vacuum dehydration; S300: adding the reactive plasticizer, MDI and IPDI and mixing them evenly to form a premixed system, wherein the NCO% content in the premixed system reaches 1.8% to 2.9%; S400: The premixed system is placed in a nitrogen environment and heated to 70° C. to 90° C. for full reaction; S500: adding the remaining components into the premixed system, heating to 90° C. to 110° C., evacuating until no bubbles are generated, and discharging the material to obtain the moisture-curable polyurethane resin.
3. The manufacturing process according to claim 2, characterized in that: The polyester polyol has a molecular weight of 4000-8000, a hydroxyl value of 45-50 mgKOH / g, and an acid value of 0.78-0.92 mgKOH / g.
4. The manufacturing process according to claim 3, characterized in that: The polyester polyol comprises the following components in parts by weight: 12-16 parts of terephthalic acid; Isophthalic acid 5.6-8.4 parts; Sebacic acid 6.7-8.2 parts Adipic acid 5.9-7.6 parts; Ethylene glycol 10.4-13.6 parts 9.6-11.5 parts of dedeoxycholic acid; The step S100 also includes the following: S101: Add all components into a reactor to melt, introduce nitrogen, heat to 160°C~180°C, and react fully; S102: distilling out the water generated in the reactor; S103: raising the temperature to 170° C. to 230° C., adjusting the vacuum degree in the reactor to 500 Pa, and evaporating the unreacted components, side reactions and water to obtain the polyester polyol.
5. A composite system for implementing the manufacturing process according to any one of claims 1 to 4, characterized in that: include: A first unwinding mechanism, used for unwinding the reflective bead-embedded film; A second unwinding mechanism, used for unwinding the substrate; A hot melt coating device, connected to the first unwinding mechanism, comprises a vacuum hot melt adhesive melter, a vacuum conveying pipe and a hot melt coating head, for melting and conveying the moisture-curing polyurethane resin and hot-melt coating the moisture-curing polyurethane resin on the reflective bead-embedded film; A pressing device, used for cold pressing or hot pressing the composite material; The humidification curing mechanism provides an environment with a humidity of 50% to 80% for curing moisture-curing polyurethane resin.
6. The composite system according to claim 5, characterized in that The hot melt coating head adopts a dual-channel design, the coating amount is controlled within 25 g / m2 to 150 g / m2, and the coating amount accuracy is controlled within ±3 g / m2.
7. The composite system according to claim 5, characterized in that: The vacuum hot melt glue melting machine adopts a melting cylinder type glue melting method, the glue melting efficiency is not less than 240Kg / h, and the temperature control range is 120℃-280℃.
8. The composite system according to claim 5, characterized in that: The temperature of the pressing mechanism is controlled at 50° C.-150° C., and the composite pressure is controlled at 0.3 MPa-0.7 MPa.
9. The composite system according to claim 5, characterized in that: The temperature of the pressing mechanism is controlled at 20° C.-150° C., and the composite pressure is controlled at 0.3 MPa-0.7 MPa.
10. The composite system according to claim 9, characterized in that The substrate is TC cloth or chemical fiber cloth or flame retardant cloth containing polyurethane coating.