Near-infrared highly-reflective PVC material and preparation method therefor

Abstract

The present application relates to a near-infrared highly-reflective PVC material and a preparation method therefor. The near-infrared highly-reflective PVC material comprises a base fabric layer and PVC coatings coating both sides of the base fabric layer. Raw materials for preparing the PVC coatings comprise in parts by weight: 95 parts of PVC paste resin, 45-65 parts of diisononyl phthalate, 1-2 parts of a stabilizer, 25-40 parts of an IR pigment, 3-4 parts of a flame retardant, and 1-2 parts of other auxiliaries, the IR pigment being obtained by modifying BASF Sicopal Black L0095 with dioctyl phthalate and EO / PO block polyether. The preparation method comprises preparation of the base fabric layer, material coating, and curing. In the present application, the BASF Sicopal Black L0095 pigment is modified by dioctyl phthalate and EO / PO block polyether (e.g., FTRT®500L1), thereby solving the problem of incompatibility between the pigment and a plasticizer. The optimized formula design ensures that the reflectivity of the material can stably reach or exceed 40%, which is particularly important to application scenarios (such as building film structures, tent houses, and military materials) in which efficient thermal insulation and cooling performance is required.

Description

Near-infrared high-reflection PVC material and preparation method thereof TECHNICAL FIELD

[0001] The present application relates to the technical field of PVC coating, in particular to a near-infrared high-reflection PVC material and a preparation method thereof. BACKGROUND

[0002] PVC coating materials have been widely used in diversified fields such as building membrane structures, tent houses and military materials due to their multifunctionality. However, with the deepening of the public's awareness of environmental protection and energy saving, higher thermal protection standards are required for the application of PVC materials in specific fields, especially their role as thermal barriers. This demand aims to enhance the reflection capability of PVC materials to infrared radiation, especially in the energy-intensive near-infrared band (700-2500 nm), by significantly improving the reflectivity to a higher level, such as from the current less than 10% to about 40%, thereby achieving significant thermal insulation and cooling effects.

[0003] The innovative development of infrared reflective PVC materials usually involves key components such as PVC paste resin, plasticizer and IR pigment. However, a significant technical challenge emerges during actual production: the alkaline IR pigment is incompatible with the commonly used ortho-phthalic plasticizer. This incompatibility not only limits the full play of material performance, but also poses a considerable obstacle to the smoothness of the entire preparation process. Therefore, while pursuing high-efficiency infrared reflection performance, how to solve this compatibility problem has become a key technical problem that needs to be overcome in the research and application fields of infrared reflective PVC materials. SUMMARY

[0004] To solve the above problems, the present application provides a near-infrared high-reflection PVC material and a preparation method thereof, aiming to effectively improve the incompatibility between alkaline IR pigment and ortho-phthalic plasticizer by optimizing the formula design, while striving to improve the reflection performance of PVC materials in the near-infrared band, ensuring that the reflectivity can stably reach or exceed 40%, to meet the demand for high-efficiency thermal insulation and cooling performance in fields such as building membrane structures, tent houses and military materials.

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

[0006] A near-infrared high-reflection PVC material, comprising a base cloth layer and a PVC coating layer coated on both sides of the base cloth layer, the preparation raw materials of the PVC coating layer comprise the following components in terms of weight fraction:

[0007] IR pigment is a BASF Sicopal Black L0095 pigment modified by dioctyl phthalate and EO / PO block polyether.

[0008] By adopting the above technical solution: the BASF Sicopal Black L0095 pigment is modified by dioctyl phthalate and EO / PO block polyether (such as ), the common incompatibility problem between the alkaline IR pigment and the phthalic plasticizer is effectively solved, and the modification not only promotes the uniform dispersion of the pigment in the PVC system, but also enhances the adhesion between the pigment and the substrate, thereby improving the overall stability and durability of the material.

[0009] The optimized formula design, especially the introduction of the modified IR pigment, significantly improves the reflection performance of the PVC material in the near-infrared wave band. By accurately controlling the proportion of each component and the modification process, the reflectivity of the material can be stabilized to reach or exceed 40%, which is particularly important for applications such as building membrane structures, tent houses, and military materials that require high-efficiency heat insulation and cooling performance.

[0010] Possible reasons are analyzed:

[0011] Dioctyl phthalate (DOP) as a common plasticizer, its molecular structure is similar to that of diisononyl phthalate (DINP) and other phthalic plasticizers. Modifying BASF Sicopal Black L0095 pigment with DOP may help form a thin film on the surface of the pigment that is compatible with the plasticizer in the PVC system, thereby reducing the interfacial tension between the pigment and the plasticizer, improving the dispersion and compatibility of the pigment in the PVC.

[0012] EO / PO block polyether (such as ) as a surfactant or compatibilizer, its unique molecular structure can interact with the pigment and other components in the PVC system. This modification may enhance the wettability of the pigment particle surface, promote the uniform dispersion of the pigment in the PVC matrix, reduce the agglomeration of the pigment particles, and improve the adhesion between the pigment and the PVC substrate.

[0013] The optimized formula design precisely controls the weight fraction of PVC paste resin, plasticizer, stabilizer, IR pigment, flame retardant, and other additives, so that each component can interact with each other to achieve the best performance balance.

[0014] Preferably, the raw materials for preparing the IR pigment include, by weight percentage: BASF Sicopal Black L0095 pigment 90-95% Dioctyl phthalate 4.5-9.0% EO / PO block polyether 0.5-1%

[0015] and are prepared by the following preparation method:

[0016] The mixing container is cleaned, and a predetermined amount of BASF Sicopal Black L0095 pigment is first added and slightly stirred to ensure that the pigment is evenly spread on the bottom of the container;

[0017] Then, dioctyl phthalate is gradually added while stirring at low speed to avoid excessive dust or local agglomeration;

[0018] After the pigment and dioctyl phthalate are evenly mixed, the EO / PO block polyether is slowly added to the mixing container and stirred at high speed to ensure thorough mixing;

[0019] During or after mixing, samples are taken for infrared reflection performance testing to ensure compliance.

[0020] By using the above technical solution: not only solves the incompatibility problem between the pigment and the plasticizer, but also significantly improves the near-infrared reflection performance of the pigment, laying a solid foundation for the preparation of high-performance near-infrared high-reflective PVC materials.

[0021] Preferably, the EO / PO block polyether is

[0022] By using the above technical solution: As a kind of EO / PO block polyether, it can effectively interact with PVC resin and other additives, promote the uniform dispersion of the pigment in the PVC system, thereby avoiding the agglomeration and precipitation of the pigment particles, and improving the stability and dispersibility of the pigment;

[0023] 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 adhere to the PVC substrate, and improve the adhesion and durability of the coating.

[0024] Preferably, the flame retardant is at least one of triphenyl phosphate and triisopropyl phenyl phosphate.

[0025] By adopting the above technical scheme: the phosphoric acid triphenyl ester and the phosphoric acid triisopropyl phenyl ester can decompose at high temperature to produce phosphorus-containing compounds such as phosphoric acid, which can catalyze the carbonization process of the PVC material and form a dense carbonized layer covering the surface of the material. This carbonized layer not only effectively insulates oxygen and heat, but also prevents the escape of flammable gas, thereby significantly improving the flame retardant performance of the PVC material.

[0026] These two flame retardants have good compatibility with PVC resin and can be uniformly dispersed in the PVC material, reducing the agglomeration and precipitation of the flame retardant particles, ensuring the stable existence and continuous effect of the flame retardant in the material, and further improving the flame retardant effect of the material.

[0027] Compared with other types of flame retardants, the phosphoric acid triphenyl ester and the phosphoric acid triisopropyl phenyl ester have less effect on the physical properties and processing performance of the PVC material, and they do not significantly reduce the strength, toughness or processing flowability of the material, so the original excellent performance of the PVC material can be maintained.

[0028] Preferably, the other additives include one or more of adhesives, UV-resistant agents, and titanium white.

[0029] By adopting the above technical scheme, the adhesion, weather resistance and aesthetic appearance of the PVC material can be significantly improved, and the addition of these additives makes the PVC material not only maintain excellent near-infrared reflection performance, but also have better practicality and market competitiveness.

[0030] In a second aspect, the application provides a preparation method of a near-infrared high-reflection PVC material, which adopts the following technical scheme:

[0031] A preparation method of a near-infrared high-reflection PVC material, the preparation steps comprising:

[0032] S1, preparation of the base cloth layer: selecting polyester fiber as the material and preparing the base cloth layer by a biaxial warp knitting machine;

[0033] S2, material coating: mixing the PVC paste resin, diisononyl phthalate, stabilizer, IR pigment, flame retardant and other additives, and stirring uniformly to prepare a PVC coating slurry, and then uniformly coating the prepared PVC coating slurry on both sides of the base cloth layer prepared in step S1 by dipping;

[0034] S3, curing: sending the base cloth layer coated with the PVC coating into a curing oven for curing, and after curing, cutting and trimming the material to obtain the near-infrared high-reflection PVC material.

[0035] By adopting the above technical scheme: the near-infrared high-reflective PVC material prepared has not only excellent near-infrared reflective performance, but also good physical performance, weather resistance and aesthetic degree. The material has wide application prospects in the fields of tent houses, building membrane structures, military protection and the like, and can meet the needs of different fields for high-performance and high-safety materials.

[0036] Preferably, the porosity of the base cloth layer in step S1 is 10-12%.

[0037] By adopting the above technical scheme: it is beneficial for the PVC coating slurry to better penetrate into the fiber gaps of the base cloth layer, forming a more firm combination. The enhanced adhesion not only can improve the durability of the coating, but also can prevent the coating from peeling or cracking and the like during use.

[0038] Preferably, the viscosity of the PVC coating slurry in step S2 is 4000-4500 mPa·s.

[0039] By adopting the above technical scheme: the viscosity of 4000-4500 mPa·s ensures that the PVC coating slurry can be uniformly and smoothly covered on the base cloth layer during coating, avoiding the problems of over-thickness, under-thickness or unevenness of the coating, which helps to improve the uniformity and aesthetic degree of the coating, and at the same time ensures the thickness and performance of the coating.

[0040] Preferably, the curing temperature in step S3 is 160-180℃, and the curing time is 1-2h.

[0041] By adopting the above technical scheme: under this curing condition, the PVC coating can form a dense and uniform structure, has excellent physical performance, weather resistance and chemical stability, and 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.

[0042] In summary, the present application includes at least one beneficial technical effect:

[0043] 1. The present application solves the incompatibility problem between the pigment and the plasticizer by modifying the BASF Sicopal Black L0095 pigment with dioctyl phthalate and EO / PO block polyether (such as ), promotes the uniform dispersion of the pigment in the PVC system, significantly improves the near-infrared reflective performance of the material, and the optimized formula design ensures that the reflectivity of the material can stably reach or exceed 40%, which is particularly important for application scenarios (such as building membrane structures, tent houses and military materials) that require high-efficiency heat insulation and cooling performance;

[0044] 2. In addition to excellent near-infrared reflection performance, the present application also significantly improves the adhesion, weather resistance and aesthetics of the PVC material by adding adhesives, UV-resistant agents, titanium white and other additives. The introduction of flame retardants (such as triphenyl phosphate and triisopropyl phenyl phosphate) significantly improves the flame retardant performance of the material, ensuring the safety of the material during use. These comprehensive performance improvements make the PVC material not only maintain high performance, but also have better practicality and market competitiveness;

[0045] 3. The preparation method provided by the present 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 the production efficiency, but also ensures the quality and stability of the final product. At the same time, the process flow of impregnation coating and high temperature curing makes the PVC coating firmly adhere to the base fabric layer, forming a composite material with excellent performance. DETAILED DESCRIPTION

[0046] The present application is further described in conjunction with the following examples. The raw materials used in the present application are commercially available common materials, except for the special description below.

[0047] Preparation Example 1-2

[0048] An IR pigment, its raw materials and the corresponding amount (kg) are shown in Table 1 below.

[0049] Table 1

[0050] Among them, the EO / PO block polyether is

[0051] and is prepared by the following preparation method:

[0052] In a clean and dry mixing container, first add the predetermined amount of BASF Sicopal Black L0095 pigment, and stir slightly to ensure that the pigment is evenly spread on the bottom of the container. Then, gradually add dioctyl phthalate while stirring at low speed to avoid excessive dust or local agglomeration.

[0053] After the pigment and plasticizer dioctyl phthalate are preliminarily mixed evenly, slowly add the EO / PO block polyether to the mixing container. Since the addition amount of EO / PO block polyether is small, special attention should be paid to its uniform dispersion. Use ultrasonic dispersion to mix the mixture thoroughly, detect and adjust.

[0054] During or after mixing, samples are taken for performance testing of infrared reflectance to ensure that the quality meets the requirements.

[0055] Preparation Example 3

[0056] An IR pigment is prepared in a manner basically the same as in Example 1, except that an equal amount of HTK-6096 is used instead.

[0057] Preparation Example 4

[0058] An IR pigment is prepared using the same method as in Basic Preparation Example 1, except that an equal amount of KJ-1800 superdispersant is used instead.

[0059] Example 1

[0060] A near-infrared high reflectivity PVC material, the raw materials and application amounts (kg) of which are shown in Table 2 below.

[0061] Table 2

[0062] Other additives consist of adhesives and UV stabilizers, with the adhesive being... 6119, UV protectant is UV-360;

[0063] And it was prepared by the following method:

[0064] S1. Preparation of the base fabric layer: Polyester fiber is selected as the material and the base fabric layer is obtained by biaxial warp knitting machine. The porosity of the base fabric layer is 10%.

[0065] S2. Material Coating: Mix PVC paste resin, diisononyl phthalate, stabilizer, IR pigment prepared by Preparation Example 1, flame retardant and other additives, and stir evenly at an appropriate temperature to prepare PVC coating slurry. The viscosity of PVC coating slurry is 4200 mPa·s. Apply the prepared PVC coating slurry evenly to both sides of the base fabric layer prepared in step S1 by impregnation. The coating thickness of both the upper and lower sides is 3 mm.

[0066] S3. Curing: The PVC-coated base fabric layer is placed in a curing oven and cured at 160°C for 1.5 hours. After curing, the material is cut, trimmed and other post-processing operations are performed to obtain the final product.

[0067] Examples 2-6

[0068] A near-infrared high reflectivity PVC material, the preparation method and raw materials used are basically the same as in Example 1, the only difference is that the amount of each raw material in the PVC coating preparation is different, as shown in Table 3 below;

[0069] Table 3

[0070] Examples 7-9

[0071] A near-infrared high-reflective PVC material was prepared according to the method of Example 1, except that the source of the IR pigment used in the preparation of the PVC coating was different. The details are shown in Table 4 below:

[0072] Table 4

[0073] Example 10

[0074] A near-infrared high-reflective PVC material was prepared according to the method of Example 1, except that the PVC coating was additionally added with other IR pigment BASF Sicotan Brown K2711 when changing the color. The details are shown in Table 5 below:

[0075] Table 5

[0076] Example 11

[0077] A near-infrared high-reflective PVC material was prepared according to the method of Example 1, except that the PVC coating was additionally added with other common pigment BASF Sicotan Brown K2711 when changing the color. The details are shown in Table 6 below:

[0078] Table 6

[0079] Comparative Example 1

[0080] A near-infrared high-reflective PVC material was prepared according to the method of Example 1, except that the PVC coating was additionally added with other IR pigment BASF Sicopal Black L0095 which was not modified.

[0081] Performance Test

[0082] I. Near-infrared reflectance test:

[0083] The materials prepared from the examples and comparative examples were cut into 5 square samples of 3x3 cm in size in the same area, and the reflectivity in the range of 700-2500 nm was measured using a TEMP 2000A portable infrared emissivity / reflectivity tester. The test results were averaged.

[0084] The performance test results are shown in Table 7 below:

[0085] Table 7

[0086] From the data analysis of Table 7, it can be seen that the near-infrared high-reflectivity PVC materials prepared in Examples 1-6 have a reflectivity of more than 40% in the near-infrared 700-2500 nm wavelength range. 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 amount is not the more the better. From Examples 5-6, it can be seen that further increasing the content of IR pigments increases the reflectivity of the prepared material samples in the 700-2500 nm wavelength range.

[0087] As for the near-infrared high-reflectivity PVC materials prepared in Examples 7-9, except for Example 9, their reflectivity in the near-infrared 700-2500 nm range reached 40%, especially Example 7, which reached 49%, and can be used as a preferred example. In Example 9, the preparation raw material of the modified IR pigment used KJ-1800 super dispersant to replace an equal amount of , whose reflectivity is only 38%;

[0088] , KJ-1800 is a super dispersant, , and KJ-1800 may differ in chemical structure, intermolecular forces, etc., affecting the uniformity and stability of the IR pigment in the PVC system, and thus affecting the reflectivity of the material.

[0089] In addition to dispersibility, the interaction between the modified IR pigment and the PVC substrate is also an important factor affecting the reflectivity. Different modifiers may change the properties of the pigment surface, affecting its adhesion and compatibility with the PVC substrate. KJ-1800 super dispersant may not be able to effectively enhance the adhesion of the pigment to the PVC substrate as , resulting in the detachment or migration of some pigments during processing or use, reducing the reflectivity.

[0090] In Examples 10 and 11, in order to change the color of the prepared near-infrared high-reflectivity PVC material, other colored pigments are often mixed. In Example 10, two infrared reflective IR pigments are mixed to prepare, while in Example 11, ordinary pigments are mixed with infrared reflective IR pigments to prepare. From the test results, the reflectivity of the near-infrared high-reflectivity PVC material in Example 11 is only 14%, which shows that the infrared reflective IR pigment will lose its infrared reflective function after being mixed with ordinary pigments. Therefore, color matching must use all infrared reflective IR pigments.

[0091] In Comparative Example 1, we used an unmodified IR pigment (BASF Sicopal Black L0095 pigment) as one of the raw materials for preparing the near-infrared high-reflectance PVC material, and the experimental results showed that the reflectivity of the near-infrared high-reflectance PVC material prepared therefrom was only 22%, which was significantly lower than expected, and verified the obvious incompatibility problem between the infrared reflective IR pigment and the phthalate plasticizer.

[0092] II. Flame Retardancy Test:

[0093] In the flame retardancy test, the test was carried out in accordance with the GB / T 5455-1997 standard.

[0094] The specific test results are shown in Table 8 below.

[0095] Table 8

[0096] Through data analysis of Table 8, it can be seen that the near-infrared high-reflectance PVC materials prepared in Examples 1 to 11 and Comparative Example 1 all exhibit excellent performance in the flame retardancy test, successfully reaching the B1 flame retardant level standard.

[0097] The above are modifications or obvious technical inspirations that can be made by those skilled in the art after reading this specification without creative contribution, but as long as they are within the scope of the claims of the present application, they should be protected by the Patent Law.

Claims

1. A near-infrared high-reflectance PVC material, characterized in that, The PVC coating layer is prepared from the following components by weight: The IR pigment is prepared by modifying BASF Sicopal Black L0095 pigment with dioctyl phthalate and EO / PO block polyether.

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

3. The near-infrared high-reflecting PVC material according to claim 1 or 2, characterized in that, The EO / PO block polyether is 500L1.

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

5. The near-infrared high reflective PVC material according to claim 1, characterized in that, The other auxiliary agents include one or more of a binder, an anti-UV agent, and titanium white.

6. A process for the production of a near-infrared highly reflective PVC material according to any one of claims 1 to 5, characterized in that The preparation steps include: S1. Preparation of the base cloth layer: polyester fibers are selected as the material, and a base cloth layer is prepared by a biaxial warp knitting machine; S2. Material coating: the PVC paste resin, diisononyl phthalate, stabilizer, IR pigment, flame retardant, and other auxiliary agents are mixed and uniformly stirred to prepare a PVC coating slurry, and the prepared PVC coating slurry is uniformly coated on both sides of the base cloth layer prepared in step S1 by impregnation; S3. Curing: the base cloth layer coated with the PVC coating is sent into a curing oven for curing, and after curing is completed, the material is cut and trimmed to obtain the product.

7. The method of producing a near-infrared high-reflectance PVC material according to claim 6, characterized by, The porosity of the base cloth layer in step S1 is 10-12%.

8. The method of claim 6, wherein the near-infrared high-reflectance PVC material is prepared by adding 0.1 to 0.5 parts by weight of the near-infrared high-reflectance pigment to 100 parts by weight of a PVC resin. The viscosity of the PVC coating slurry in step S2 is 4000-4500 mPa·s.

9. The method of claim 6, wherein the near-infrared high-reflectance PVC material is prepared by adding 0.1 to 0.5 parts by weight of the near-infrared high-reflectance pigment to 100 parts by weight of a PVC resin. The curing temperature in step S3 is 160-180°C, and the curing time is 1-2 h.

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