Polyester-based composite functional master batch as well as preparation method and application thereof

Abstract

The invention provides a polyester-based composite functional master batch as well as a preparation method and application thereof. The polyester-based composite functional master batch is prepared from the following components in parts by weight: 54 to 100 parts of polyethylene glycol terephthalate-1, 4-cyclohexanedimethanol ester, 4 to 27 parts of a lubricating agent, 0.5 to 2 parts of a compatilizer, 0.5 to 10 parts of a light diffusion agent, 1 to 8 parts of a dispersing agent and 4 to 10 parts of tackifying resin. The polyester-based composite functional master batch provided by the invention is added in the process of processing and forming a polyethylene glycol terephthalate-1, 4-cyclohexanedimethanol ester-based light diffusion plate, so that the flowability and the demolding property can be improved, and the prepared product has excellent light transmittance and haze at the same time.

Description

Technical Field

[0001] The invention belongs to the technical field of polyester-based composite materials, and specifically relates to a polyester-based composite functional masterbatch and a preparation method and application thereof. Background Art

[0002] Polyester is a general term for polymers formed by polycondensation of polyols and polyacids. PET is the most representative polyester product among polyester materials. However, PET has a low glass transition temperature and is not suitable for areas with high ambient temperatures. It has a high melting point, which is not conducive to the processing and molding of materials. It has a slow crystallization rate and will undergo cold crystallization when heated, which has an adverse effect on the transparency of PET molded products. PETG is a new type of completely amorphous transparent copolyester obtained by copolymerizing PET with 1,4-cyclohexanedimethanol (CHDM) as the third monomer to partially replace ethylene glycol. It is widely used in cosmetic packaging materials, medical packaging, household appliances, high-end membrane materials, and building sheets due to its high transparency, impact resistance, weather resistance, and chemical resistance, wide processing temperature range, and being a recyclable and environmentally friendly material that meets food contact requirements.

[0003] In the automatic production of injection molding and extrusion molding, the injection molding material is required to have good fluidity and easy demoulding. In order to maintain the appearance quality and dimensional stability of the product during the sampling process of the robot arm and not affect the automatic production process, a high intrinsic viscosity is required. At the same time, in the application of household appliance covers, while ensuring high light transmittance, the strong glare and concentrated light source must be transformed into a light with uniform brightness and no strong contrast with the surrounding environment. Therefore, a polyester material with good fluidity, easy demoulding, high light transmittance and high haze is required.

[0004] CN106046736A discloses a method for preparing a polyester resin-based light diffusion composite material. The raw material formula of the polyester resin-based light diffusion composite material is composed of the following raw material components by weight: 100 parts of base resin, 0.3-1.5 parts of light diffusion agent, 0.1-0.6 parts of antioxidant, and 0.1-0.5 parts of release agent; the base resin is composed of 50%-70% of polycarbonate and 30%-50% of polyester terephthalate by weight, and the polyester terephthalate is a composition formed by PET and one or two of APET and PETG; the preparation method of the polyester resin-based light diffusion composite material provided by the technical solution is simple and easy to implement, suitable for industrial production, and greatly reduces the cost of light diffusion materials for LEDs, but the light transmittance is low and still needs to be improved.

[0005] CN117070056A discloses a PET composite material and its application, wherein the PET composite material comprises the following components by weight: 79.5-95.5 parts of isophthalic acid modified PET plastic, 4.8-15.2 parts of organic light diffuser, and 0.9-5.1 parts of nucleating agent; the mass percentage of isophthalic acid in the isophthalic acid modified PET plastic is 2.9%-31.5%; the organic light diffuser comprises at least one of acrylate polymer, ethylene-vinyl acetate copolymer, and silicone. The technical scheme adds a specific amount of organic light diffuser and nucleating agent to PET plastic with a specific isophthalic acid content, so that the obtained PET composite material has a higher total light transmittance and bending modulus. The LED lampshade made by using the composite material has not only a high total light transmittance, but also a light diffusion uniformity evaluation grade above the intermediate level, but the haze and light transmittance are still low and need to be improved.

[0006] The materials used to prepare home appliance diffusion plates in the existing solutions still have problems such as low toughness, environmental pollution, small processing range, and great processing difficulty. At the same time, the commonly used preparation method is to blend trace additives with the base material and extrude granules, and then use them for injection molding and extrusion processing. The process is complicated and the performance is unstable. The particle-type light diffuser used is easy to agglomerate in the matrix, which increases the haze while greatly reducing the light transmittance.

[0007] Therefore, it is necessary to develop a composite functional masterbatch that can increase the fluidity and demoulding properties of PETG resin and make the product have high light transmittance and high haze at the same time. Summary of the invention

[0008] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a polyester-based composite functional masterbatch and its preparation method and application. Adding the polyester-based composite functional masterbatch in the processing and molding of polyethylene terephthalate-1,4-cyclohexanedimethanol-based light diffuser plates can improve fluidity and demoulding properties, so that the prepared product has excellent light transmittance and haze.

[0009] To achieve this object, the present invention adopts the following technical solutions:

[0010] In a first aspect, the present invention provides a polyester-based composite functional masterbatch, wherein the polyester-based composite functional masterbatch comprises the following components in parts by weight: 54 to 100 parts (e.g., 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts or 95 parts, etc.) of polyethylene terephthalate-1,4-cyclohexanedimethanol ester, 4 to 27 parts (e.g., 7 parts, 10 parts, 13 parts, 16 parts, 19 parts, 22 parts or 25 parts, etc.) of lubricant , 0.5-2 parts of compatibilizer (for example 0.7 parts, 0.9 parts, 1.1 parts, 1.3 parts, 1.5 parts, 1.7 parts or 1.9 parts, etc.), 0.5-10 parts of light diffusing agent (for example 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.), 1-8 parts of dispersant (for example 2 parts, 3 parts, 4 parts, 5 parts, 6 parts or 7 parts, etc.) and 4-10 parts of tackifying resin (for example 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.).

[0011] In the present invention, lubricants and light diffusers are added to the polyester-based composite functional masterbatch, which effectively avoids the agglomeration phenomenon during the twin-screw extrusion process when the light diffuser is added alone. The polyester-based composite functional masterbatch is added in the processing and molding of the polyethylene terephthalate-1,4-cyclohexanedimethanol-based light diffuser plate so that the prepared product has excellent light transmittance and haze at the same time, improving the problem that high haze and high light transmittance cannot be combined. The polyester-based composite functional masterbatch is added to the PETG resin for production and processing, which reduces the viscosity of the PETG resin, improves the processing fluidity of the PETG resin, is easy to form, and reduces the processing temperature at the same time, can avoid the decomposition of the material at high temperature and save energy consumption; adding the polyester-based composite functional masterbatch to the PETG resin can improve the demoulding property of the product, and the product can be smoothly separated from the mold without damage, deformation or residue, etc., which greatly improves the production efficiency and product quality. The polyester-based composite functional masterbatch can be directly physically mixed with the PETG resin for processing and production, without the need for twin-screw granulation into mixed material particles for further processing, which greatly reduces the material preparation cost and improves production efficiency.

[0012] Preferably, the polyethylene terephthalate-1,4-cyclohexanedimethanol ester comprises PETG and / or PCTG.

[0013] In the present invention, the PETG is obtained by copolymerization of terephthalic acid, ethylene glycol and 1,4-cyclohexanedimethanol, wherein the molar amount of the diol residue is 100%, and the molar amount of the 1,4-cyclohexanedimethanol residue is ≤50%; the PCTG is obtained by copolymerization of terephthalic acid, ethylene glycol and 1,4-cyclohexanedimethanol, wherein the molar amount of the diol residue is 100%, and the molar amount of the 1,4-cyclohexanedimethanol residue is greater than 50%.

[0014] Preferably, the molar amount of 1,4-cyclohexanedimethanol residues in the polyethylene terephthalate-1,4-cyclohexanedimethanol ester is 20% to 65%, such as 25%, 30%, 35%, 40%, 45%, 50%, 55% or 60%, etc., based on the molar amount of diol residues as 100%.

[0015] In the present invention, the introduction of the 1,4-cyclohexanedimethanol monomer destroys the symmetrical structure of the polyethylene terephthalate molecular chain, slows down the crystallization rate, reduces the crystallinity, and has high transparency. In addition, the cyclic structure of 1,4-cyclohexanedimethanol in the molecular chain enhances the rigidity of the material, so that polyethylene terephthalate-1,4-cyclohexanedimethanol ester has excellent transparency and rigidity.

[0016] Preferably, the intrinsic viscosity of the polyethylene terephthalate-1,4-cyclohexanedimethanol ester is 0.56 to 0.8 dL / g, for example, 0.59 dL / g, 0.62 dL / g, 0.65 dL / g, 0.68 dL / g, 0.71 dL / g, 0.74 dL / g, 0.77 dL / g, 0.78 dL / g or 0.8 dL / g.

[0017] Preferably, the light transmittance of a 5 mm thick sheet made of polyethylene terephthalate-1,4-cyclohexanedimethanol is ≥89.0% (e.g., 90%, 91% or 92%, etc.), and the haze is ≤1.0% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%, etc.).

[0018] In this aspect, the transmittance and haze of the sheet made of polyethylene terephthalate-1,4-cyclohexanedimethanol with a thickness of 5 mm are obtained by testing with an integrating sphere transmittance and haze tester.

[0019] Preferably, the lubricant includes any one of oleamide, erucamide, pentaerythritol stearate, glyceryl stearate, polyethylene glycol, polyethylene wax, montan wax or zinc stearate, or a combination of at least two thereof.

[0020] In this aspect, the lubricant can be evenly dispersed in the polyester-based composite functional masterbatch, reducing the internal friction between molecules in the material during processing, thereby improving the flow properties of the material. At the same time, part of the lubricant acts on the contact surface between the material and the processing equipment to form a film, reducing the friction and adhesion between the material and the equipment, thereby improving the processing performance of the material and making it easier to demold from the mold.

[0021] Preferably, the compatibilizer includes any one of a maleic anhydride grafted polymer, a silane coupling agent or an epoxy group-containing compatibilizer, or a combination of at least two thereof.

[0022] In the present invention, the compatibilizer can enhance the compatibility of polyethylene terephthalate-1,4-cyclohexanedimethanol with other components.

[0023] Preferably, the light diffuser includes an organic light diffuser and / or an inorganic light diffuser.

[0024] Preferably, the organic light diffuser includes silicone resin microspheres and / or methyl silicone oil.

[0025] Preferably, the inorganic light diffuser includes any one of SiO2, TiO2, calcium carbonate, barium sulfate or aluminum oxide, or a combination of at least two thereof.

[0026] Preferably, the average particle size of the inorganic light diffuser is 1 to 3.5 μm, for example, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm, 2.0 μm, 2.2 μm, 2.4 μm, 2.6 μm, 2.8 μm, 3.0 μm, 3.2 μm or 3.4 μm.

[0027] Preferably, the dispersant comprises dimethylsiloxane.

[0028] Preferably, the tackifying resin includes any one of hydrogenated rosin, terpene resin, C5 petroleum resin, C9 petroleum resin or C5 / C9 copolymerized petroleum resin, or a combination of at least two thereof.

[0029] In the present invention, the addition of the tackifying resin can avoid the phenomenon that the melt cannot be cut into pellets due to the low viscosity of the material at the rear end of the extruder pelletizing.

[0030] Preferably, the polyester-based composite functional masterbatch also includes 0.1 to 0.3 parts by weight of an antioxidant, for example, 0.12 parts by weight, 0.14 parts by weight, 0.16 parts by weight, 0.18 parts by weight, 0.2 parts by weight, 0.22 parts by weight, 0.24 parts by weight, 0.26 parts by weight or 0.28 parts by weight.

[0031] Preferably, the antioxidant comprises any one of a hindered phenol antioxidant, a phosphite antioxidant or a thiodipropionic acid diester, or a combination of at least two thereof.

[0032] In the present invention, adding the antioxidant can delay or inhibit the progress of the polymer oxidation process, thereby preventing the aging of the polymer and extending its service life.

[0033] In a second aspect, the present invention provides a method for preparing a polyester-based composite functional masterbatch as described in the first aspect, the preparation method comprising the following steps: mixing polyethylene terephthalate-1,4-cyclohexanedimethanol, a lubricant, a compatibilizer, a light diffuser, a dispersant and a tackifying resin, and granulating to obtain the polyester-based composite functional masterbatch.

[0034] Preferably, the preparation method specifically comprises the following steps:

[0035] (1) Polyethylene terephthalate-1,4-cyclohexanedimethanol ester and a dispersant are uniformly mixed in a high-speed mixer, and then a light diffuser, a compatibilizer and an antioxidant are sequentially added and mixed to form a premix.

[0036] (2) feeding the premix obtained in step (1) into the main feed port of the twin-screw extruder, feeding the lubricant and the tackifying resin into the side feed port, extruding, and granulating to obtain the polyester-based composite functional masterbatch.

[0037] Preferably, the mixing temperature of the high mixer in step (1) is 40-70° C. (e.g., 45° C., 50° C., 55° C., 60° C. or 65° C., etc.), the rotation speed is 150-300 rpm (e.g., 170 rpm, 190 rpm, 210 rpm, 230 rpm, 250 rpm, 270 rpm or 290 rpm, etc.), and the mixing time is 15-75 min (e.g., 25 min, 35 min, 45 min, 55 min or 65 min, etc.).

[0038] Preferably, the twin-screw extruder in step (2) is provided with twelve zones, the lubricant is fed from the side feed port of zone five, and the tackifying resin is fed from the side feed port of zone eight.

[0039] Preferably, the temperature of zone 1 of the twin-screw extruder in step (2) is 20-40°C (e.g., 22°C, 24°C, 26°C, 28°C, 30°C, 32°C, 34°C, 36°C or 38°C, etc.), the temperature of zone 2 is 160-220°C (e.g., 170°C, 180°C, 190°C, 200°C or 210°C, etc.), the temperature of zone 3 is 180-240°C (e.g., 190°C, 200°C, 210°C, 220°C or 230°C, etc.), and the temperature of zone 4 is 180-250°C (e.g., 190°C, 200°C, 210°C, 220°C, 230°C or 240°C). The temperature of zone 5 is 180-250℃ (for example, 190℃, 200℃, 210℃, 220℃, 230℃ or 240℃, etc.), the temperature of zone 6 is 180-250℃ (for example, 190℃, 200℃, 210℃, 220℃, 230℃ or 240℃, etc.), the temperature of zone 7 is 180-240℃ (for example, 190℃, 200℃, 210℃, 220℃ or 230℃, etc.), the temperature of zone 8 is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.), the temperature of zone 9 is 180-250℃ (for example, 190℃, 200℃, 210℃, 220℃, 230℃ or 240℃, etc.), the temperature of zone 7 is 180-240℃ (for example, 190℃, 200℃, 210℃, 220℃ or 230℃, etc.), the temperature of zone 8 is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.), The temperature is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.), the temperature of zone 10 is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.), the temperature of zone 11 is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.), the temperature of zone 12 is 200-240℃ (205℃, 210℃, 215℃, 220℃, 225℃, 230℃ or 235℃, etc.) 35°C, etc.), the die temperature is 210-260°C (215°C, 220°C, 225°C, 230°C, 235°C, 240°C, 245°C, 250°C or 255°C, etc.), the main feeding frequency is 5-10Hz (for example, 5.5Hz, 6Hz, 6.5Hz, 7Hz, 7.5Hz, 8Hz, 8.5Hz, 9Hz or 9.5Hz, etc.), and the screw speed is 200-350rpm (for example, 220rpm, 240rpm, 260rpm, 280rpm, 300rpm, 320rpm or 340rpm, etc.).

[0040] In a third aspect, the present invention provides a polyester composition, comprising a polyester matrix resin and a polyester-based composite functional masterbatch as described in any one of claims 1 to 6.

[0041] Preferably, the polyester composition comprises, by weight: 90 to 99 parts (for example, 91 parts, 92 parts, 93 parts, 94 parts, 95 parts, 96 parts, 97 parts or 98 parts, etc.) of a polyester matrix resin and 1 to 10 parts (for example, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.) of the polyester-based composite functional masterbatch.

[0042] Preferably, the polyester matrix resin includes polyethylene terephthalate-1,4-cyclohexanedimethanol, and more preferably includes PETG and / or PCTG.

[0043] In a fourth aspect, the present invention provides a use of the polyester-based composite functional masterbatch as described in the first aspect or the polyester composition as described in the third aspect in the preparation of a light diffuser plate.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] In the present invention, the polyester-based composite functional masterbatch is added with a lubricant and a light diffuser, which effectively avoids the agglomeration phenomenon that occurs during the twin-screw extrusion process when the light diffuser is added alone. The polyester-based composite functional masterbatch is added during the processing and molding of the polyethylene terephthalate-1,4-cyclohexanedimethanol-based light diffuser plate, so that the obtained product has excellent light transmittance and haze at the same time, improving the problem that high haze and high light transmittance cannot be combined. The polyester-based composite functional masterbatch is added to the PETG resin for production and processing, which can reduce the viscosity of the PETG resin, improve the processing fluidity and demoulding properties, and greatly improve the production efficiency and product quality. The polyester-based composite functional masterbatch can be directly physically mixed with the PETG resin for processing and production, without the need for twin-screw granulation into mixed material particles for further processing, which greatly reduces the material preparation cost and improves the production efficiency. The light diffuser plate made by adding the polyester-based composite functional masterbatch has a demoulding force of ≤8 Bar, a light transmittance of ≥85%, and a haze of ≥20%. Preferably, the demoulding force is ≤7.2 Bar, the light transmittance of ≥89%, and the haze of ≥95%. DETAILED DESCRIPTION

[0046] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0047] Some of the raw materials for the following examples and comparative examples are as follows:

[0048] PETG, brand name Honggang HG-1701, intrinsic viscosity 0.78dL / g, the transmittance of the sheet with a thickness of 5mm is 89%, and the haze is 1.2%;

[0049] PETG, brand SKK2012, intrinsic viscosity 0.78dL / g, the transmittance of the sheet with a thickness of 5mm is 90%, and the haze is 1%;

[0050] PCTG, brand SK JN200, has an intrinsic viscosity of 0.74 dL / g. The light transmittance of a sheet with a thickness of 5 mm is 90% and the haze is 1%.

[0051] Example 1

[0052] The present embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The polyester-based composite functional masterbatch includes the following components: 59.8kg of PETG (Honggang HG-1701), 15kg of lubricant (pentaerythritol stearate), 1kg of compatibilizer (ADR4468), 8kg of light diffuser (organic silicone resin microspheres with an average particle size of 1.3μm, brand JTK-101, manufactured by Zhongtong Chemical), 8kg of dispersant (dimethylsiloxane, viscosity at 25°C is 100CS), 0.1kg of antioxidant 1010, 0.1kg of antioxidant 168 and 8kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials).

[0053] The polyester-based composite functional masterbatch is prepared by the following method:

[0054] (1) After PETG and dispersant were mixed in a high-speed mixer for 10 minutes, light diffuser, compatibilizer, antioxidant 1010, and antioxidant 168 were added in sequence and mixed. The processing parameters of the high-speed mixer were: speed 200 rpm, mixing temperature 60° C., mixing time 60 min, to form a premix;

[0055] (2) feeding the premix obtained in step (1) into the main feed port of a twin-screw extruder, feeding the lubricant into the side feed port of zone five, and feeding the tackifying resin into the side feed port of zone eight. The processing parameters of the twin-screw extruder are as follows: the processing temperature of each zone is: zone one temperature 25°C, zone two temperature 160°C, zone three temperature 200°C, zone four temperature 215°C, zone five temperature 220°C, zone six temperature 230°C, zone seven temperature 230°C, zone eight temperature 230°C, zone nine temperature 230°C, zone ten temperature 230°C, zone eleven temperature 220°C, zone twelve temperature 220°C, die head temperature 220°C, main feeding frequency 5 Hz, screw speed 200 rpm, extruder model CJWH35 extruder manufactured by Changzhou Jwell Intelligent Chemical Equipment Co., Ltd., extrusion granulation to obtain the polyester-based composite functional masterbatch.

[0056] The light diffuser plate is prepared by mixing 2 parts by weight of the polyester-based composite functional masterbatch and 98 parts by weight of PETG (Honggang HG-1701) in a high-speed mixer, and then injection molding to obtain a light diffuser plate of 100 mm×100 mm×5 mm.

[0057] Example 2

[0058] The present embodiment provides a polyester-based composite functional masterbatch, a preparation method thereof, and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the polyester-based composite functional masterbatch comprises the following components: 64.8 kg of PETG (Honggang HG-1701), 10 kg of lubricant (zinc stearate, pentaerythritol stearate and glyceryl stearate in a mass ratio of 1:2:2), 1 kg of compatibilizer (ADR4468), 10 kg of light diffuser (silicone resin microspheres with an average particle size of 1.3 μm, brand JTK-101, manufactured by Zhongtong Chemical), 8 kg of dispersant (dimethylsiloxane, viscosity of 100 CS at 25°C), 0.1 kg of antioxidant 1010, 0.1 kg of antioxidant 168 and 6 kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials), and other conditions are the same as those in the embodiment 1.

[0059] Example 3

[0060] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the mass of PETG (Honggang HG-1701) is adjusted to 57.8 kg, the mass of the light diffuser (silicone resin microspheres, with an average particle size of 1.3 μm, brand JTK-101, and manufactured by Zhongtong Chemical) is adjusted to 10 kg, and other conditions are the same as in Example 1.

[0061] Example 4

[0062] The present embodiment provides a polyester-based composite functional masterbatch, a preparation method thereof, and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the polyester-based composite functional masterbatch comprises the following components: 50.8 kg of PETG (Honggang HG-1701), 20 kg of lubricant (zinc stearate, pentaerythritol stearate and glyceryl stearate in a mass ratio of 7:5:8), 1 kg of compatibilizer (ADR4468), 10 kg of light diffuser (organic silicone resin microspheres with an average particle size of 1.3 μm, brand JTK-101, manufactured by Zhongtong Chemical), 8 kg of dispersant (dimethylsiloxane, viscosity of 100 CS at 25°C), 0.1 kg of antioxidant 1010, 0.1 kg of antioxidant 168 and 10 kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials), and other conditions are the same as those in the embodiment 1.

[0063] Example 5

[0064] The present embodiment provides a polyester-based composite functional masterbatch, a preparation method thereof, and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the polyester-based composite functional masterbatch comprises the following components: 66.8 kg of PETG (Honggang HG-1701), 10 kg of lubricant (zinc stearate), 1 kg of compatibilizer (ADR4468), 8 kg of light diffuser (organic silicone resin microspheres with an average particle size of 1.3 μm, brand JTK-101, manufactured by Zhongtong Chemical), 8 kg of dispersant (dimethylsiloxane, viscosity at 25°C is 100CS), 0.1 kg of antioxidant 1010, 0.1 kg of antioxidant 168 and 6 kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials), and other conditions are the same as those in the embodiment 1.

[0065] Example 6

[0066] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the mass of PETG (Honggang HG-1701) is adjusted to 69.8 kg, the mass of the lubricant (pentaerythritol stearate) is adjusted to 5 kg, and other conditions are the same as those in Example 1.

[0067] Example 7

[0068] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the mass of PETG (Honggang HG-1701) is adjusted to 49.8 kg, the mass of the lubricant (pentaerythritol stearate) is adjusted to 25 kg, and the other conditions are the same as those in Example 1.

[0069] Example 8

[0070] The present embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the mass of PETG (Honggang HG-1701) is adjusted to 62.8 kg, the mass of the light diffuser (silicone resin microspheres, with an average particle size of 1.3 μm, brand JTK-101, and manufactured by Zhongtong Chemical) is adjusted to 5 kg, and the other conditions are the same as those in the embodiment 1.

[0071] Example 9

[0072] The present embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the mass of PETG (Honggang HG-1701) is adjusted to 67.3 kg, the mass of the light diffuser (silicone resin microspheres, with an average particle size of 1.3 μm, brand JTK-101, and manufactured by Zhongtong Chemical) is adjusted to 0.5 kg, and the other conditions are the same as those in the embodiment 1.

[0073] Example 10

[0074] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The difference between this embodiment and Example 1 is that PETG (Honggang HG-1701) is replaced with PCTG (SK JN200) of the same quality, and other conditions are the same as those in Example 1.

[0075] Embodiment 11

[0076] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that PETG (Honggang HG-1701) is replaced with PETG (SKK2012) of the same quality, and other conditions are the same as those in Example 1.

[0077] Example 12

[0078] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the light diffuser (silicone resin microspheres, with an average particle size of 1.3 μm) is replaced with a light diffuser of the same mass (SiO2, with an average particle size of 3.5 μm), and other conditions are the same as those in Example 1.

[0079] Example 13

[0080] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the light diffuser (silicone resin microspheres with an average particle size of 1.3 μm) is replaced with a light diffuser of the same mass (barium sulfate with an average particle size of 3.5 μm), and other conditions are the same as those in Example 1.

[0081] Embodiment 14

[0082] This embodiment provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate. The only difference between this embodiment and Example 1 is that the light diffuser (silicone resin microspheres with an average particle size of 1.3 μm) is replaced with a light diffuser of the same mass (calcium carbonate with an average particle size of 3.5 μm), and other conditions are the same as those in Example 1.

[0083] Embodiment 15

[0084] The present embodiment provides a polyester-based composite functional masterbatch, a preparation method thereof, and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the polyester-based composite functional masterbatch comprises the following components: 59.8 kg of PETG (Honggang HG-1701), 15 kg of lubricant (pentaerythritol stearate), 0.5 kg of compatibilizer (ADR4468), 8 kg of light diffuser (organic silicone resin microspheres with an average particle size of 1.3 μm, brand JTK-101, manufactured by Zhongtong Chemical), 6.6 kg of dispersant (dimethylsiloxane, with a viscosity of 100 CS at 25°C), 0.05 kg of antioxidant 1010, 0.05 kg of antioxidant 168, and 10 kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials), and other conditions are the same as those in the embodiment 1.

[0085] Example 16

[0086] The present embodiment provides a polyester-based composite functional masterbatch, a preparation method thereof, and a light diffuser plate. The only difference between the present embodiment and the embodiment 1 is that the polyester-based composite functional masterbatch comprises the following components: 59.8 kg of PETG (Honggang HG-1701), 15 kg of lubricant (pentaerythritol stearate), 2 kg of compatibilizer (ADR4468), 10 kg of light diffuser (organic silicone resin microspheres with an average particle size of 1.3 μm, brand JTK-101, manufactured by Zhongtong Chemical), 8 kg of dispersant (dimethylsiloxane, with a viscosity of 100 CS at 25°C), 0.2 kg of antioxidant 1010, 0.1 kg of antioxidant 168, and 4 kg of tackifying resin (C9 petroleum resin, brand HP-140, manufactured by Henghe Materials), and other conditions are the same as those in the embodiment 1.

[0087] Comparative Example 1

[0088] This comparative example provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate, which differs from Example 1 only in that no light diffuser is added, the mass of PETG (Honggang HG-1701) is adjusted to 67.8 kg, and other conditions are the same as Example 1.

[0089] Comparative Example 2

[0090] This comparative example provides a polyester-based composite functional masterbatch and a preparation method thereof and a light diffuser plate, which differs from Example 1 only in that no lubricant is added, the mass of PETG (Honggang HG-1701) is adjusted to 74.8 kg, and other conditions are the same as Example 1.

[0091] The light diffuser plates provided in Examples 1-16 and Comparative Examples 1-2 were subjected to the following performance tests.

[0092] (1) Demolding force: Under the same injection molding conditions, the polyester-based composite functional masterbatch was injection molded into a light diffuser plate, and the force of the ejector pin of the injection molding machine was recorded.

[0093] (2) Helix: The polyester-based composite functional masterbatch was injection molded under the same injection molding conditions to prepare the light diffuser plate, and the length of the Archimedean spiral process in the mold was recorded.

[0094] (3) Light transmittance: The light transmittance test was performed according to ASTM D1003-00.

[0095] (4) Haze: The haze test was conducted according to ASTM D1003-00.

[0096] The test results are shown in Table 1 below.

[0097] Table 1

[0098]

[0099]

[0100] It can be seen from the contents of Table 1 that the demolding force of the light diffuser plate provided in Examples 1-16 is ≤8Bar, the transmittance is ≥85%, and the haze is ≥20%. Adding the polyester-based composite functional masterbatch of the present invention to the processing and molding of the polyethylene terephthalate-1,4-cyclohexanedimethanol-based light diffuser plate can improve the fluidity and demolding properties, so that the obtained product has excellent transmittance and haze at the same time.

[0101] Compared with Example 1, if the quality of the lubricant is low (Example 6), the fluidity of the injection molding material is reduced, the demoulding force required for the light diffuser plate is large, and defects are easily formed on the surface of the light diffuser plate during the molding process, resulting in unstable quality of the light diffuser plate.

[0102] Compared with Example 1, if the quality of the lubricant is too high (Example 7), the transmittance of the prepared light diffuser plate is reduced. Too much lubricant may destroy the continuous phase structure of the material, making the internal structure of the material unstable. It is impossible to maintain sufficient pressure and speed during the molding process, and internal defects are easily formed.

[0103] Compared with Example 1, if the quality of the light diffuser is low (Example 9), the haze of the prepared light diffuser plate is seriously low, and it is impossible to convert the strong glare and concentrated light source into light with uniform brightness and no strong contrast.

[0104] Compared with Example 1, if the light diffuser is not added (Comparative Example 1), the haze of the prepared light diffuser plate is extremely low, and the problem of uniform light diffusion cannot be effectively solved.

[0105] Compared with Example 1, if no lubricant is added (Comparative Example 2), the light diffuser plate cannot effectively guarantee the effective and smooth demoulding of the product processing and the stability of the product size during the preparation process, which increases the defective rate of the product and the processing cost.

[0106] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate a polyester-based composite functional masterbatch and its preparation method and application, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A polyester-based composite functional masterbatch, characterized in that: The polyester-based composite functional masterbatch comprises the following components in parts by weight: 54-100 parts of polyethylene terephthalate-1,4-cyclohexanedimethanol ester, 4-27 parts of lubricant, 0.5-2 parts of compatibilizer, 0.5-10 parts of light diffuser, 1-8 parts of dispersant and 4-10 parts of tackifying resin.

2. The polyester-based composite functional masterbatch according to claim 1, characterized in that: The polyethylene terephthalate-1,4-cyclohexanedimethanol ester includes PETG and / or PCTG; Preferably, the molar amount of the 1,4-cyclohexanedimethanol residue in the polyethylene terephthalate-1,4-cyclohexanedimethanol ester is 20% to 65% based on the molar amount of the diol residue as 100%; Preferably, the intrinsic viscosity of the polyethylene terephthalate-1,4-cyclohexanedimethanol ester is 0.56 to 0.8 dL / g; Preferably, the light transmittance of the sheet made of polyethylene terephthalate-1,4-cyclohexanedimethanol and having a thickness of 5 mm is ≥89.0%, and the haze is ≤1.0%.

3. The polyester-based composite functional masterbatch according to claim 1 or 2, characterized in that: The lubricant comprises any one or a combination of at least two of oleamide, erucamide, pentaerythritol stearate, glyceryl stearate, polyethylene glycol, polyethylene wax, montan wax or zinc stearate; Preferably, the compatibilizer includes any one of a maleic anhydride grafted polymer, a silane coupling agent or a compatibilizer containing an epoxy group, or a combination of at least two thereof.

4. The polyester-based composite functional masterbatch according to any one of claims 1 to 3, characterized in that: The light diffuser includes an organic light diffuser and / or an inorganic light diffuser; Preferably, the organic light diffuser comprises silicone resin microspheres and / or methyl silicone oil; Preferably, the inorganic light diffuser includes any one or a combination of at least two of SiO2, TiO2, calcium carbonate, barium sulfate or aluminum oxide; Preferably, the average particle size of the inorganic light diffusing agent is 1 to 3.5 μm; Preferably, the dispersant comprises dimethylsiloxane.

5. The polyester-based composite functional masterbatch according to any one of claims 1 to 4, characterized in that: The tackifying resin includes any one of hydrogenated rosin, terpene resin, C5 petroleum resin, C9 petroleum resin or C5 / C9 copolymerized petroleum resin or a combination of at least two thereof.

6. The polyester-based composite functional masterbatch according to any one of claims 1 to 5, characterized in that: The polyester-based composite functional masterbatch further comprises 0.1 to 0.3 parts by weight of an antioxidant; Preferably, the antioxidant comprises any one of a hindered phenol antioxidant, a phosphite antioxidant or a thiodipropionic acid diester, or a combination of at least two thereof.

7. A method for preparing a polyester-based composite functional masterbatch according to any one of claims 1 to 6, characterized in that: The preparation method comprises the following steps: mixing polyethylene terephthalate-1,4-cyclohexanedimethanol, a lubricant, a compatibilizer, a light diffuser, a dispersant and a tackifying resin, and granulating to obtain the polyester-based composite functional masterbatch.

8. The preparation method according to claim 7, characterized in that: The preparation method specifically comprises the following steps: (1) mixing polyethylene terephthalate-1,4-cyclohexanedimethanol and a dispersant in a high-speed mixer, and then sequentially adding a light diffuser, a compatibilizer and an antioxidant to form a premix; (2) feeding the premix obtained in step (1) into a twin-screw extruder from a main feed port, feeding a lubricant and a tackifying resin into the side feed port, extruding, and granulating to obtain the polyester-based composite functional masterbatch; Preferably, the mixing temperature of the high-speed mixer in step (1) is 40-70° C., the rotation speed is 150-300 rpm, and the mixing time is 15-75 min. Preferably, the twin-screw extruder in step (2) is provided with twelve zones, the lubricant is fed from the side feed port of zone five, and the tackifying resin is fed from the side feed port of zone eight; Preferably, the temperature of zone 1 of the twin-screw extruder in step (2) is 20-40°C, the temperature of zone 2 is 160-220°C, the temperature of zone 3 is 180-240°C, the temperature of zone 4 is 180-250°C, the temperature of zone 5 is 180-250°C, the temperature of zone 6 is 180-250°C, the temperature of zone 7 is 180-240°C, the temperature of zone 8 is 200-240°C, the temperature of zone 9 is 200-240°C, the temperature of zone 10 is 200-240°C, the temperature of zone 11 is 200-240°C, the temperature of zone 12 is 200-240°C, the temperature of the die head is 210-260°C, the main feeding frequency is 5-10HZ, and the screw speed is 200-350rpm.

9. A polyester composition, characterized in that The polyester composition comprises a polyester matrix resin and a polyester-based composite functional masterbatch as described in any one of claims 1 to 6; Preferably, the polyester composition comprises, by weight: 90 to 99 parts of polyester matrix resin, and 1 to 10 parts of the polyester-based composite functional masterbatch; Preferably, the polyester matrix resin includes polyethylene terephthalate-1,4-cyclohexanedimethanol, and more preferably includes PETG and / or PCTG.

10. Use of the polyester-based composite functional masterbatch according to any one of claims 1 to 6 or the polyester composition according to claim 9 in the preparation of a light diffuser plate.

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