A near-infrared high-reflection PVC material and its preparation method

Abstract

The present application relates to a near-infrared highly reflective PVC material and a preparation method thereof. The near-infrared highly reflective PVC material comprises a base fabric layer and a PVC coating applied on both sides of the base fabric layer. The PVC coating is prepared from the following raw materials, by weight: 95 parts PVC paste resin, 45-65 parts diisononyl phthalate, 1-2 parts stabilizer, 25-40 parts IR pigment, 3-4 parts flame retardant, and 1-2 parts other additives; the IR pigment is BASF Sicopal Black L0095 modified with dioctyl phthalate and EO / PO block polyether. The preparation method includes preparation of a base fabric layer, material coating, and curing. This application addresses the incompatibility issue between the pigment and the plasticizer by modifying BASF Sicopal Black L0095 IR pigment with dioctyl phthalate and EO / PO block polyether (such as FTRT®500L1). The optimized formula design ensures that the material's reflectivity can stably reach or exceed 40%, which is particularly important for applications requiring efficient thermal insulation and cooling performance (such as architectural membrane structures, tents, and military materials).

Description

Technical Field

[0001] The present application relates to the technical field of PVC coatings, and in particular to a near-infrared high-reflective PVC material and a preparation method thereof. Background Art

[0002] Due to its versatility, PVC coating materials have been widely used in diverse fields, including architectural membrane structures, tents, and even military materials. However, with the deepening awareness of environmental protection and energy conservation, higher thermal protection standards are being proposed for PVC applications in specific areas, especially its role as a thermal barrier. This demand aims to enhance PVC's ability to reflect infrared radiation, especially the energy-intensive near-infrared band (700-2500 nanometers). By significantly increasing reflectivity to higher levels, such as from less than 10% to approximately 40%, significant insulation and cooling effects can be achieved.

[0003] The innovative development of infrared-reflective PVC materials typically incorporates key components such as PVC paste resin, plasticizer, and IR pigment. However, a significant technical challenge has emerged during actual production: incompatibility between alkaline IR pigments and commonly used ortho-phthalic plasticizers. This incompatibility not only limits the full performance of the material but also poses a significant obstacle to the smooth execution of the entire production process. Therefore, while pursuing high-efficiency infrared reflectivity, resolving this compatibility issue has become a key technical challenge that needs to be overcome in the development and application of infrared-reflective PVC materials. Summary of the Invention

[0004] To solve the above problems, the present application provides a near-infrared highly reflective PVC material and a preparation method thereof, aiming to effectively improve the incompatibility between alkaline IR pigments and ortho-phthalic plasticizers by optimizing the formula design, while at the same time striving to enhance the reflective performance of the PVC material in the near-infrared band, ensuring that the reflectivity can stably reach or exceed 40%, so as to meet the requirements for efficient thermal insulation and cooling performance in fields such as architectural membrane structures, tents and military materials.

[0005] In the first aspect, the present application provides a near-infrared high-reflection PVC material adopts the following technical solution:

[0006] A near-infrared high-reflection PVC material, characterized in that it includes a base fabric layer and a PVC coating coated on both sides of the base fabric layer, wherein the raw materials for preparing the PVC coating include the following components in parts by weight:

[0007]

[0008]

[0009] The IR pigment is BASF Sicopal Black L0095 modified with dioctyl phthalate and EO / PO block polyether.

[0010] By adopting the above technical solution: BASF Sicopal Black L0095 IR pigment is treated with dioctyl phthalate and EO / PO block polyether (such as The modification of 500L1) effectively solves the common incompatibility problem between basic IR pigments and ortho-phthalic plasticizers. This modification not only promotes the uniform dispersion of the pigment in the PVC system, but also strengthens the binding force between the pigment and the substrate, thereby improving the overall stability and durability of the material.

[0011] The optimized formula design, especially the introduction of modified IR pigments, significantly improves the reflective performance of PVC materials in the near-infrared band. By precisely controlling the proportions of each component and the modification process, the reflectivity of the material is ensured to stably reach or exceed 40%. This is particularly important for application scenarios that require efficient thermal insulation and cooling properties, such as architectural membrane structures, tents and military materials.

[0012] Analyze the possible reasons:

[0013] Dioctyl phthalate (DOP) is a common plasticizer with a molecular structure similar to that of phthalate plasticizers such as diisononyl phthalate (DINP). Modifying IR pigments with DOP may help form a film on the pigment surface that is compatible with the plasticizer in the PVC system, thereby reducing the interfacial tension between the pigment and the plasticizer and improving the dispersibility and compatibility of the pigment in PVC.

[0014] EO / PO block polyether (such as 500L1) As a surfactant or compatibilizer, its unique molecular structure can simultaneously interact well with the pigment and other components in the PVC system. This modification may promote the uniform dispersion of the pigment in the PVC matrix by enhancing the wettability of the pigment particle surface, while reducing the agglomeration of the pigment particles and improving the binding force between the pigment and the PVC substrate;

[0015] The optimized formula design precisely controls the weight proportions of PVC paste resin, plasticizer, stabilizer, IR pigment, flame retardant and other additives, allowing the components to work synergistically with each other to achieve the best performance balance.

[0016] Preferably, the modified preparation raw material of IR pigment comprises, by weight percentage:

[0017] BASF Sicopal Black L0095 90-95%

[0018] Dioctyl phthalate 4.5-9.0%

[0019] EO / PO block polyether 0.5-1%

[0020] And it is prepared by the following preparation method:

[0021] Clean the mixing container and first add the predetermined amount of BASF Sicopal Black L0095 pigment and stir gently to ensure that the pigment is evenly spread on the bottom of the container;

[0022] Then gradually add dioctyl phthalate while stirring at a low speed to avoid excessive dust or local agglomeration; after the pigment and plasticizer are preliminarily mixed, slowly add the EO / PO block polyether to the mixing container and stir at a high speed ultrasonically to mix them thoroughly;

[0023] During or after the mixing process, samples are taken for infrared reflection performance testing to ensure that they meet the requirements.

[0024] By adopting the above technical solution, not only the incompatibility problem between the pigment and the plasticizer is solved, but also the near-infrared reflection performance of the pigment is significantly improved, laying a solid foundation for the preparation of high-performance near-infrared high-reflection PVC materials.

[0025] Preferably, the EO / PO block polyether is 500L1.

[0026] By adopting the above technical solution: As a type of EO / PO block polyether, 500L1 can effectively interact with PVC resin and other additives to promote the uniform dispersion of pigments in the PVC system, thereby avoiding the agglomeration and precipitation of pigment particles and improving the stability and dispersibility of the pigments.

[0027] In addition, it can also enhance the interfacial bonding force between the pigment and the PVC substrate. It can form a thin film on the surface of the pigment particles, improve the interaction between the pigment and the PVC resin, make the pigment more firmly attached to the PVC substrate, and improve the adhesion and durability of the coating.

[0028] Preferably, the flame retardant is at least one of triphenyl phosphate and triisopropylphenyl phosphate.

[0029] By adopting the above technical solution: triphenyl phosphate and triisopropylphenyl phosphate can decompose at high temperature to produce phosphoric acid and other phosphorus-containing compounds. These compounds can catalyze the carbonization process of the PVC material, forming a dense carbonized layer covering the surface of the material. This carbonized layer can not only effectively isolate oxygen and heat, but also prevent the escape of combustible gases, thereby significantly improving the flame retardant properties of the PVC material;

[0030] These two flame retardants have good compatibility with PVC resin and can be evenly dispersed in the PVC material, reducing the agglomeration and precipitation of flame retardant particles, ensuring the stable presence and continuous effect of the flame retardant in the material, and further improving the flame retardant effect of the material;

[0031] At the same time, compared with other types of flame retardants, triphenyl phosphate and triisopropylphenyl phosphate have less effect on the physical properties and processing properties of PVC materials. They will not significantly reduce the strength, toughness or processing fluidity of the material, so they can maintain the original excellent properties of PVC materials.

[0032] Preferably, the other additives include one or more of a binder, an anti-UV agent, and titanium dioxide.

[0033] By adopting the above technical solution, the comprehensive properties of PVC materials, such as adhesion, weather resistance and aesthetics, can be significantly improved. The addition of these additives enables PVC materials to have better practicality and market competitiveness while maintaining excellent near-infrared reflection performance.

[0034] In a second aspect, the present application provides a method for preparing a near-infrared highly reflective PVC material using the following technical solution: A method for preparing a near-infrared highly reflective PVC material, the preparation steps comprising:

[0035] S1, preparation of base fabric layer: select polyester fiber as material, and knit the base fabric layer by biaxial warp knitting machine;

[0036] S2. Material coating: PVC paste resin, diisononyl phthalate, stabilizer, modified IR pigment, flame retardant, and other additives are mixed in a certain proportion and stirred evenly at an appropriate temperature to prepare a PVC coating slurry. The prepared PVC coating slurry is evenly coated on both sides of the base fabric layer prepared in step S1 by dipping;

[0037] S3, curing: the base fabric layer coated with the PVC coating is sent to a curing oven for curing. After curing is completed, the material is subjected to post-processing operations such as cutting and trimming.

[0038] By adopting this technical solution, the resulting near-infrared highly reflective PVC material not only exhibits excellent near-infrared reflectivity, but also possesses excellent physical properties, weather resistance, and aesthetics. This material has broad application prospects in fields such as tents, architectural membrane structures, and military protection, meeting the demand for high-performance, high-safety materials in various fields.

[0039] Preferably, the porosity of the base fabric layer in step S1 is 10-12%.

[0040] By adopting the above technical solution: it is beneficial for the PVC coating slurry to better penetrate into the fiber gaps of the base fabric layer, forming a stronger bond. This enhanced adhesion can not only improve the durability of the coating, but also prevent the coating from peeling or cracking during use.

[0041] Preferably, the viscosity of the PVC coating slurry in step S2 is 4000-4500 mPa·s.

[0042] By adopting the above technical solution: the viscosity of 4000-4500mPa·s ensures that the PVC coating slurry can be evenly and smoothly covered on the base fabric layer during the coating process, avoiding the problem of excessively thick, thin or uneven coating, which helps to improve the uniformity and aesthetics of the coating while ensuring the thickness and performance of the coating.

[0043] Preferably, in step S3, the curing temperature is 160-180° C., and the curing time is 1-2 hours.

[0044] By adopting the above technical solution: under this curing condition, the PVC coating can form a dense and uniform structure with excellent physical properties, weather resistance and chemical stability. At the same time, since the pigments and other additives are fully dispersed and fixed during the curing process, the near-infrared reflective performance of the coating can also be well maintained and improved.

[0045] In summary, this application includes at least one beneficial technical effect:

[0046] 1. This application is to BASF Sicopal Black L0095 IR pigment by dioctyl phthalate and EO / PO block polyether (such as The modified treatment of 500L1) solves the incompatibility problem between pigments and plasticizers, promotes the uniform dispersion of pigments in the PVC system, and significantly improves the near-infrared reflectivity of the material. The optimized formula design ensures that the material's reflectivity can stably reach or exceed 40%, which is particularly important for applications requiring efficient thermal insulation and cooling performance (such as architectural membrane structures, tents and military materials).

[0047] 2. In addition to excellent near-infrared reflectivity, this application also significantly improves the adhesion, weather resistance, and aesthetics of the PVC material by adding binders, UV inhibitors, titanium dioxide, and other additives. The introduction of flame retardants (such as triphenyl phosphate and triisopropylphenyl phosphate) significantly improves the material's flame retardancy, ensuring the material's safety during use. These comprehensive performance improvements enable the PVC material to maintain high performance while also possessing greater practicality and market competitiveness.

[0048] 3. The preparation method provided in this application ensures the uniformity, adhesion and durability of the coating by precisely controlling the porosity of the base fabric layer (10-12%), the viscosity of the PVC coating slurry (4000-4500 mPa·s), and the curing temperature and time (160-180°C, 1-2h). The optimization of these process parameters not only improves production efficiency, but also ensures the quality and stability of the final product. At the same time, the process flow of dip coating and high-temperature curing enables the PVC coating to be firmly attached to the base fabric layer, forming a composite material with excellent performance. DETAILED DESCRIPTION

[0049] The present application is further described in detail below with reference to the examples. Except for the special instructions below, the raw materials used in the present application are all common commercially available materials.

[0050] Preparation Example 1-2

[0051] The following table lists the raw materials and dosage (kg) of an IR pigment.

[0052]

[0053] Among them, EO / PO block polyether is 500L1;

[0054] And it is prepared by the following preparation method:

[0055] In a clean, dry mixing container, first add the predetermined amount of BASF Sicopal Black L0095 pigment and stir gently to ensure that the pigment is evenly spread on the bottom of the container. Then, gradually add dioctyl phthalate while stirring at a low speed to avoid excessive dust or local agglomeration.

[0056] After the pigment and plasticizer are preliminarily mixed, slowly add the EO / PO block polyether into the mixing container. Since the amount of EO / PO block polyether added is small, special attention should be paid to its dispersion uniformity. Use ultrasonic dispersion to fully mix the mixture, test and adjust it;

[0057] During or after the mixing process, samples are taken for performance testing of infrared reflectance to ensure that the quality meets the requirements.

[0058] Preparation Example 3

[0059] An IR pigment, the preparation method of which is the same as that of Preparation Example 1, except that HTK-6096 is used in equal amounts instead of 500L1.

[0060] Preparation Example 4

[0061] An IR pigment, the preparation method of which is the same as that of Preparation Example 1, except that KJ-1800 hyperdispersant is used in equal amounts instead of 500L1.

[0062] Example 1

[0063] A near-infrared highly reflective PVC material, its preparation raw materials and corresponding dosage (kg) are shown in the following table.

[0064]

[0065] Among them, other additives are composed of adhesives and anti-UV agents. The adhesive is Beep 6119, anti-UV agent is UV-360;

[0066] And it is prepared by the following preparation method:

[0067] S1. Preparation of base fabric layer: polyester fiber is selected as the material and knitted by a biaxial warp knitting machine to obtain a base fabric layer, the porosity of the base fabric layer is 10%;

[0068] S2. Material coating: PVC paste resin, diisononyl phthalate, stabilizer, IR pigment prepared in Preparation Example 1, flame retardant, and other additives were mixed in a certain proportion and stirred uniformly at an appropriate temperature to prepare a PVC coating slurry. The viscosity of the PVC coating slurry was 4200 mPa·s. The prepared PVC coating slurry was evenly coated on both sides of the base fabric layer prepared in step S1 by dipping. The coating thickness on both sides was 3 mm.

[0069] S3, curing: the base fabric layer coated with the PVC coating is sent to a curing oven for curing at 160° C. for 1.5 hours. After the curing is completed, the material is subjected to post-processing operations such as cutting and trimming.

[0070] Examples 2-6

[0071] A near-infrared high-reflection PVC material, the preparation method and raw materials used are the same as those in Example 1, the only difference being that the amounts of the various components in the preparation of the PVC coating are different, as shown in the table below.

[0072]

[0073]

[0074] Examples 7-9

[0075] A near-infrared high-reflection PVC material, the preparation method of which is the same as that of Example 1, the only difference being that the source of the IR pigment used in the preparation of the PVC coating is different. The specific details are shown in the table below:

[0076] Group Source of IR pigments used Example 7 Prepared from Preparation Example 2 Example 8 Prepared from Preparation Example 3 Example 9 Prepared from Preparation Example 4

[0077] Example 10

[0078] A near-infrared high-reflective PVC material is prepared by the same method as in Example 1, except that an additional IR pigment, BASF Sicotan Brown K2711, is added to the PVC coating when the color is changed. The specific details are shown in the table below:

[0079]

[0080] Example 11

[0081] A near-infrared high-reflection PVC material, the preparation method of which is the same as that of Example 1, except that another common pigment BASF Sicotan Brown K2711 is additionally added to the PVC coating when changing the color matching. The specific details are shown in the table below:

[0082]

[0083]

[0084] Comparative Example 1

[0085] A near-infrared high-reflection PVC material is prepared by the same method as in Example 1, except that the IR pigment used in the raw materials for preparing the PVC coating is not modified.

[0086] Performance Testing

[0087] 1. Near infrared reflection test:

[0088] The materials prepared in the examples and comparative examples were cut into 5 square samples of 3×3 cm in the same area. The reflectivity in the range of 700-2500 nm was measured using a TEMP 2000A portable infrared emissivity / reflectivity meter, and the test results were averaged.

[0089] The performance test results are shown in the following table:

[0090]

[0091] From the data analysis of the above table, it can be seen that the near-infrared high-reflective PVC materials prepared in Examples 1-6 can achieve a reflectivity of more than 40% in the near-infrared wavelength range of 700-2500nm. From Examples 2-3, it can be seen that as the amount of diisononyl phthalate increases, the reflectivity also increases. However, from the data of Example 4, it can be seen that the higher the amount, the better. From Examples 5-6, it can be seen that further increasing the content of IR pigment increases the reflectivity of the prepared material samples in the wavelength range of 700-2500nm.

[0092] As for the near-infrared high-reflection PVC materials prepared in Examples 7-9, except for Example 9, the reflectivity in the near-infrared range of 700-2500nm reached 40%, especially Example 7, which reached 49%, which can be used as a preferred example. In Example 9, the raw materials for the preparation of the modified IR pigment used KJ-1800 superdispersant were replaced in equal amounts. 500L1, its reflectivity is only 38%;

[0093] 500L1 is an EO / PO block polyether dispersant, while KJ-1800 is a hyperdispersant. There may be differences between 500L1 and KJ-1800 in terms of chemical structure and intermolecular forces, which may affect the dispersion uniformity and stability of IR pigments in the PVC system, and thus affect the reflective properties of the material;

[0094] In addition to dispersibility, the interaction between modified IR pigments and PVC substrates is also an important factor affecting reflective performance. Different modifiers may change the properties of the pigment surface, thereby affecting its binding force and compatibility with the PVC substrate. KJ-1800 hyperdispersant may not be as effective as 500L1 effectively enhances the bonding force between the pigment and the PVC substrate, causing some pigments to fall off or migrate during processing or use, reducing the reflectivity.

[0095] In Examples 10 and 11, in order to change the color of the prepared near-infrared high-reflection PVC material, pigments of other colors are often mixed. In Example 10, the same infrared-reflecting IR pigment is used, while in Example 11, ordinary pigments are used for mixing. From the test results, the reflectivity of the near-infrared high-reflection PVC material in Example 11 is only 14%. It can be seen that the infrared-reflecting IR pigment loses its infrared reflective function when mixed with ordinary pigments. Therefore, the color matching must use only infrared-reflecting IR pigments;

[0096] In Comparative Experiment 1, we used an unmodified IR pigment as one of the raw materials for preparing near-infrared high-reflection PVC material. The experimental results showed that the reflectivity of the near-infrared high-reflection PVC material obtained in this way was only 22%, which was significantly lower than expected and verified the obvious incompatibility between infrared-reflective IR pigments and ortho-phthalic plasticizers.

[0097] 2. Flame retardancy test:

[0098] In the flame retardancy test, the test was carried out in accordance with GB / T 5455-1997 standard.

[0099] The specific test results are shown in the table below.

[0100]

[0101]

[0102] By analyzing the data in the above table, it can be seen that the near-infrared high-reflection PVC materials prepared in Examples 1 to 11 and Comparative Example 1 all showed excellent performance in the flame retardant performance test and successfully reached the B1 flame retardant grade standard.

[0103] The above are all modifications that a person skilled in the art can make to this embodiment as needed after reading this specification, which do not contribute creatively or solutions that obviously constitute technical inspiration. However, as long as they are within the scope of the claims of this application, they should be protected by patent law.

Claims

1. A near-infrared high-reflection PVC material, characterized in that: The invention comprises a base fabric layer and a PVC coating applied on both sides of the base fabric layer, wherein the raw materials for preparing the PVC coating include the following components in parts by weight: 95 parts of PVC paste resin 45-65 parts of diisononyl phthalate 1-2 parts stabilizer IR pigment 25-40 parts 3-4 parts flame retardant 1-2 parts of other additives; The IR pigment is BASF Sicopal Black L0095 modified with dioctyl phthalate and EO / PO block polyether.

2. The near-infrared high-reflection PVC material according to claim 1, characterized in that: The modified preparation raw materials of the IR pigment include, by weight percentage: BASF Sicopal Black L0095 90-95% Dioctyl phthalate 4.5-9.0% EO / PO block polyether 0.5-1% And it is prepared by the following preparation method: Clean the mixing container and first add the predetermined amount of BASF Sicopal Black L0095 pigment and stir gently to ensure that the pigment is evenly spread on the bottom of the container; Then gradually add dioctyl phthalate while stirring at a low speed to avoid excessive dust or local agglomeration; After the pigment and plasticizer are preliminarily mixed, the EO / PO block polyether is slowly added to the mixing container and stirred at high speed by ultrasonication to fully mix; During or after the mixing process, samples are taken for infrared reflection performance testing to ensure that they meet the requirements.

3. The near-infrared highly reflective PVC material according to claim 1 or 2, characterized in that: The EO / PO block polyether is FTRT®500L1.

4. The near-infrared highly reflective PVC material according to claim 1, characterized in that: The flame retardant is at least one of triphenyl phosphate and triisopropylphenyl phosphate.

5. The near-infrared highly reflective PVC material according to claim 1, characterized in that: The other additives include one or more of a binder, an anti-UV agent, and titanium dioxide.

6. A method for preparing a near-infrared highly reflective PVC material, characterized in that: Its preparation steps include: S1, preparation of base fabric layer: select polyester fiber as material, and knit the base fabric layer by biaxial warp knitting machine; S2. Material coating: PVC paste resin, diisononyl phthalate, stabilizer, modified IR pigment, flame retardant, and other additives are mixed in a certain proportion and stirred evenly at an appropriate temperature to prepare a PVC coating slurry. The prepared PVC coating slurry is evenly coated on both sides of the base fabric layer prepared in step S1 by dipping; S3, curing: the base fabric layer coated with the PVC coating is sent to a curing oven for curing. After curing is completed, the material is subjected to post-processing operations such as cutting and trimming.

7. The method for preparing the near-infrared highly reflective PVC material according to claim 6, characterized in that: The porosity of the base fabric layer in step S1 is 10-12%.

8. The method for preparing the near-infrared highly reflective PVC material according to claim 6, characterized in that: The viscosity of the PVC coating slurry in step S2 is 4000-4500 mPa·s.

9. The method for preparing the near-infrared highly reflective PVC material according to claim 6, characterized in that: In step S3, the curing temperature is 160-180° C., and the curing time is 1-2 hours.

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