Additive masterbatch and its use

Abstract

It is an additive masterbatch and its use. The raw materials of the additive masterbatch include a resin base material, a high melting point additive, and a low melting point additive. Among them, the melting point of the high melting point additive is greater than 40 °C, and the melting point of the low melting point additive is 40 °C or less. The additive masterbatch effectively solves problems such as the low melting point additive masterbatch being prone to adhesion and agglomeration, the manufacturing process being complex, and being difficult to mold. The provided additive masterbatch is not prone to agglomeration, can be manufactured using an ordinary masterbatch manufacturing process, is easy to mold, and can manufacture masterbatches with different particle sizes.

Description

Technical Field

[0001] (Cross - reference to related applications) This application claims priority based on a Chinese application with the application number 202210940265.4 and the filing date of August 5, 2022, and incorporates the entire disclosure content of the Chinese application herein by reference into this application.

[0002] This application relates to the technical field of polymer materials, specifically to additive masterbatches and their use.

Background Art

[0003] When a polymer material is exposed to sunlight for a long time, it absorbs the energy of ultraviolet rays and undergoes degradation and decomposition, resulting in degradation phenomena such as discoloration, cracking, and deterioration of mechanical and electrical properties of the material, and the process of becoming unusable continuously is called photo - degradation.

[0004] Adding a light stabilizer to the production process of polymer materials can effectively reduce the above - mentioned photo - degradation reaction.

[0005] Conventional types of light stabilizers mainly include ultraviolet absorbers and hindered amine light stabilizers. Ultraviolet absorbers include benzophenone - based, benzotriazole - based, triazine - based, etc. Ultraviolet absorbers function as light stabilizers by absorbing harmful ultraviolet rays and converting them into heat for release. Hindered amine light stabilizers generate active free radicals by themselves, and further capture the free radicals generated by the degradation and decomposition of the material to function as light stabilizers. Hindered amine light stabilizers are a major advancement in the photo - stabilization of polymers and are widely used in fields such as general - purpose plastics, engineering plastics, paints, adhesives, and rubbers.

[0006] The use effect of hindered amine light stabilizers is excellent. However, since some hindered amine light stabilizers have a low melting point, it is difficult to add them during use. The solution is to manufacture such low-melting hindered amine light stabilizers as additive masterbatches so that they can be easily mixed and processed with polymer materials. However, the additive masterbatches produced in this way contain low-melting additive components, so there is a problem of agglomeration during storage, transportation, and subsequent use, which affects the normal use of downstream customers. Taking 2,2,6,6-tetramethyl-4-piperidinyl stearate (UV-3853) as an example, its melting point is only about 28°C, and it becomes white to pale yellow wax-like or oily at room temperature. As mentioned above, this is also generally manufactured as a masterbatch and provided to customers, but the manufactured masterbatch has a problem of agglomeration during storage, transportation, and subsequent use.

[0007] Regarding the technical problems in the above low-melting additive masterbatches, taking UV-3853 as an example, currently, the main solutions in the anti-degradant industry are mainly as follows. (1) Use some other processing additives such as foaming agents and adsorbents to improve the coating performance of the PP carrier for the light stabilizer UV-3853, so as to achieve the purpose of suppressing the precipitation of the light stabilizer UV-3853. However, in this method, since the adsorbent and foaming agent are introduced in a certain ratio, it may have some adverse effects on the processing process of polymer materials, such as compatibility problems. (2) Use foamed polypropylene as the carrier and absorb the 3853 liquid with foamed polypropylene to achieve the purpose of alleviating the precipitation of the light stabilizer 3853. This method has high production costs, low production efficiency, and high requirements for the processing process, so it is disadvantageous in terms of cost. (3) It is to apply a protective layer on the surface. For example, patent CN108137863A discloses 3853PP5 manufactured by adopting a co-extrusion technology with a multi-stage extruder, and a protective material layer is extruded on the surface to obtain a coating effect. However, since the cutting surface of the cutter cannot be protected, there is a phenomenon of precipitation and agglomeration in actual use.

[0008] In addition to UV-3853, other low melting point additive masterbatches also have the above-mentioned manufacturing difficulties and the problem of high adhesiveness of the masterbatch.

[0009] Therefore, this application is submitted.

Summary of the Invention

Problems to be Solved by the Invention

[0010] The main object of this application is to provide an additive masterbatch and its use, and to solve the problems of the prior art such as the low melting point additive masterbatch being prone to agglomeration and the process being complex.

Means for Solving the Problems

[0011] According to one aspect of this application to achieve the above object, an additive masterbatch is provided, the raw materials of which include a resin base material, a high melting point additive, and a low melting point additive. Among them, the melting point of the high melting point additive is greater than 40°C, and the melting point of the low melting point additive is 40°C or less.

[0012] Furthermore, the low melting point additive is a liquid or paste at room temperature, or a solid with a melting point of 40°C or less. Preferably, the melting point of the high melting point additive is greater than 80°C, more preferably greater than 100°C, still more preferably greater than 150°C, and even more preferably greater than 200°C.

[0013] Furthermore, the low melting point additive is a weather-resistant additive with a melting point of 40°C or less. Preferably, it is a light stabilizer with a melting point of 40°C or less. Preferably, the light stabilizer is a hindered amine light stabilizer and / or an ultraviolet absorber, and more preferably, it is a hindered amine light stabilizer or its composition.

[0014] Furthermore, the hindered amine light stabilizer or its composition is selected from one or more of the reaction product of bis(2,2,6,6-tetramethyl-4-piperidyl) sebacate, tert-butyl hydroperoxide and octane, 2,2,6,6-tetramethyl-4-piperidinyl stearate, the mixture of bis(1,2,2,6,6-pentamethyl-4-piperidyl) sebacate and mono(1,2,2,6,6-pentamethyl-4-piperidyl) sebacate, bis(2,2,6,6-tetramethyl-1-undecyloxy-4-yl)-carbonate, and the mixture of 2,2,6,6-tetramethyl-4-piperidinyl stearate and hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate.

[0015] Furthermore, the ultraviolet absorber is selected from one or more of benzotriazole-based ultraviolet absorbers, cyanoacrylate-based ultraviolet absorbers, benzamidine-based ultraviolet absorbers, benzophenone-based ultraviolet absorbers, hydroxyphenyltriazine-based ultraviolet absorbers, oxalic acid anilide-based ultraviolet absorbers or salicylate-based ultraviolet absorbers. More preferably, the ultraviolet absorber is selected from one or more of the reaction product of methyl 3-[3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyphenyl]propionate and PEG300, hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate, 2-ethylhexyl 2-cyano-3,3-diphenylacrylate, and N-(ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine.

[0016] Furthermore, the high melting point additive is an organic substance and / or an inorganic substance. Preferably, the high melting point additive is an additive for polymer materials. More preferably, the high melting point additive is an organic additive for polymer materials with a relative molecular mass greater than 500. Even more preferably, it is an organic additive for polymer materials with a relative molecular mass greater than 600. Even more preferably, the high melting point additive is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite, 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, and polyethylene wax. Preferably, the resin base material is a thermoplastic resin. More preferably, the thermoplastic resin is selected from one or more of polyolefin, polyester, polyether, polyketone, polyamide, polyurethane, polystyrene, high impact polystyrene, polyacrylate, polymethacrylate, polyacetal, polyacrylonitrile, polybutadiene, acrylonitrile-butadiene-styrene copolymer, acrylonitrile-styrene copolymer, acrylate-styrene-acrylonitrile copolymer, cellulose acetate butyrate, cellulose polymer, polyimide, polyamideimide, polyetherimide, polyphenylene sulfide, polyphenylene ether, polysulfone, polyether sulfone, polyvinyl chloride, polycarbonate, poly(oxymethylene), and ethylene vinyl acetate copolymer. Even more preferably, the resin base material is a polyolefin. Even more preferably, the polyolefin is selected from polypropylene and / or polyethylene.

[0017] Furthermore, based on parts by weight, the raw materials of the additive masterbatch for polymer materials include 30 to 70 parts of a resin base material, 0.1 to 30 parts of a high melting point additive, and 30 to 70 parts of a low melting point additive. More preferably, based on parts by weight, the raw materials of the additive masterbatch for polymer materials include 30 to 70 parts of a resin base material, 1 to 25 parts of a high melting point additive, and 30 to 70 parts of a low melting point additive. Even more preferably, based on parts by weight, the raw materials of the additive masterbatch for polymer materials include 40 to 60 parts of a resin base material, 1 to 20 parts of a high melting point additive, and 40 to 60 parts of a low melting point additive. Even more preferably, the weight ratio of the high melting point additive to the low melting point additive is 1:3 to 15, and most preferably, it is 1:5 to 15.

[0018] Furthermore, the low melting point additive is one or more of 2,2,6,6-tetramethyl-4-piperidinyl stearate, and a mixture of 2,2,6,6-tetramethyl-4-piperidinyl stearate and hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate. The resin base material is polyethylene or polypropylene. The high melting point additive is one or more of tris(2,4-di-tert-butylphenyl) phosphite, 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, and polyethylene wax. Preferably, the additive masterbatch comprises 1 to 20 parts of tris(2,4-di-tert-butylphenyl) phosphite, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 20 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 20 parts of 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 0.1 to 10 parts of tris(2,4-di-tert-butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 0.1 to 10 parts of tris(2,4-di-tert-butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 0.1 to 10 parts of polyethylene wax, 0.1 to 10 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione and / or tris(2,4-di-tert-butylphenyl) phosphite and / or 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin.

[0019] Furthermore, the additive masterbatch for polymer materials is formed by performing screw extrusion, granulation, drying, and cooling on the raw materials in this order. Preferably, underwater cutting granulation is adopted for granulation, and the operating temperature thereof is 190 to 230°C.

[0020] Furthermore, the particle size of the additive masterbatch for polymer materials is 1 to 5 mm.

[0021] According to another aspect of the present application, there is also provided the use of the above additive masterbatch in polymer materials.

Advantages of the Invention

[0022] The present application effectively solves problems such as low-melting-point additive masterbatches being prone to adhesion and agglomeration and having a complicated manufacturing process. The additive masterbatch manufactured according to the present application is difficult to agglomerate, and can be realized even by using ordinary equipment and processes for manufacturing the masterbatch. It is easy to operate and can manufacture additive masterbatch products with different particle sizes.

Brief Description of the Drawings

[0023] The drawings in the specification are provided for a better understanding of the present application as a part constituting the present application. The exemplary embodiments and their descriptions of the present application are for interpreting the present application and do not constitute an inappropriate limitation to the present application.

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Embodiments for Carrying Out the Invention

[0024] Unless there is a contradiction, the features in the examples and embodiments of the present application can be combined with each other. Hereinafter, the present application will be described in detail with reference to the drawings and by using examples.

[0025] As described in the background art, low-melting-point additive masterbatches are prone to adhesion and agglomeration. The conventional solutions include introducing a component capable of adsorbing the low-melting-point additive to relieve the precipitation of the additive, further reducing the risk of the masterbatch sticking and agglomerating, or extruding a further protective material layer on the surface of the masterbatch to achieve an anti-sticking and anti-agglomeration effect. The conventional solutions involve introducing a non-general adsorbent or have a complicated manufacturing process and are difficult to implement. In response to this, the present application provides a simpler and more effective solution, completely solving the problem that the additive masterbatch is prone to adhesion and agglomeration, and the provided additive masterbatch has a simple manufacturing process.

[0026] In a typical embodiment of the present application, an additive masterbatch is provided, the raw materials of which include a resin base material, a high-melting-point additive, and a low-melting-point additive, among which the melting point of the high-melting-point additive is greater than 40°C, and the melting point of the low-melting-point additive is 40°C or lower.

[0027] The reason why the low melting point additive is likely to precipitate in the resin base material of the masterbatch is not only that its melting point is low, but also related to the poor compatibility between the two. It is very difficult for the resin base material to fully cover the surface of the low melting point additive. When the temperature rises, the melting or fluidity of the low melting point additive improves, resulting in the problem of precipitation. Especially near the surface of the masterbatch, the problem of precipitation becomes more prominent. The additive masterbatch provided by the present application introduces a high melting point additive with a melting point higher than 40 °C in addition to the resin base material and the low melting point additive in its raw materials. In the manufacturing process of the masterbatch, generally steps such as screw extrusion, granulation, drying, and cooling are performed on the raw materials. However, the high melting point additive introduced in the present application can be uniformly melted and dispersed in the resin base material together with the low melting point additive at the stage of screw extrusion and granulation of the masterbatch. Then, when the processing temperature drops, the high melting point additive solidifies first and is coated on the surface of the low melting point additive, forming a protective barrier layer. Thereby, the additive masterbatch effectively suppresses the problems of adhesion and agglomeration during subsequent transportation and use.

[0028] In addition, the additive masterbatch provided by the present application only needs to adopt a normal granulation process. The inventor of the present application has conducted research and found that the particle size is also a requirement in the granulation of the masterbatch. Generally, it is necessary to make large particles or small particles according to the needs of adding different downstream materials. The particle size of the small particle masterbatch is generally (2 ± 1) × (2 ± 1) mm, and the particle size of the large particle masterbatch is generally (4 ± 1) × (4 ± 1) mm. Since the raw materials of the present application have high strength in the granulation process and can form a large melting pressure, it is guaranteed that the melt of the raw materials can smoothly pass through the small hole die to form small particle masterbatch particles. Moreover, the masterbatch has a round and swollen shape and excellent fluidity. Therefore, the particle size range of the additive masterbatch for polymer materials of the present application is wide, controllable, has good molding performance, and the formed large particle masterbatch and small particle masterbatch are shown in Figure 1 and Figure 2 respectively.

[0029] The greater the difference in melting points between the high-melting-point additive and the low-melting-point additive, the easier it is for the high-melting-point additive to form a protective film on the surface of the low-melting-point additive, and it has an effect of better promoting the prevention of agglomeration adhesion of the masterbatch. In a preferred embodiment, the low-melting-point additive of the present application is a liquid or paste at room temperature, or a solid with a melting point of 40°C or lower. The melting point of the high-melting-point additive is greater than 80°C, more preferably greater than 100°C, still more preferably greater than 150°C, and even more preferably greater than 200°C.

[0030] Preferably, the above low-melting-point additive is a weather-resistant additive with a melting point of 40°C or lower, and preferably a light stabilizer with a melting point of 40°C or lower. The above low-melting-point additive of the present application is more suitable and has a more prominent effect in alleviating problems such as agglomeration of the masterbatch. Preferably, the light stabilizer is a hindered amine light stabilizer and / or an ultraviolet absorber, and more preferably a hindered amine light stabilizer or a composition thereof.

[0031] Exemplarily, the hindered amine light stabilizer includes one or more of bis(2,2,6,6-tetramethyl-4-piperidyl) sebacate, the reaction product of tert-butyl hydroperoxide and octane (UV-123), 2,2,6,6-tetramethyl-4-piperidyl stearate (UV-3853), the mixture of bis(1,2,2,6,6-pentamethyl-4-piperidyl) sebacate and mono(1,2,2,6,6-pentamethyl-4-piperidyl) sebacate (UV-292), bis(2,2,6,6-tetramethyl-1-undecyloxy-4-yl)-carbonate, but is not limited thereto. The ultraviolet absorber includes one or more of benzotriazole-based ultraviolet absorbers, cyanoacrylate-based ultraviolet absorbers, benzamidine-based ultraviolet absorbers, benzophenone-based ultraviolet absorbers, hydroxyphenyltriazine-based ultraviolet absorbers, oxalic acid anilide-based ultraviolet absorbers or salicylate-based ultraviolet absorbers, but is not limited thereto. More preferably, the ultraviolet absorber is the reaction product of methyl 3-[3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyphenyl]propionate and PEG300 (UV-1130), hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate (UV-2908), 2-ethylhexyl 2-cyano-3,3-diphenylacrylate (UV-3039), N-(ethoxycarbonylphenyl)-N′-methyl-N′-phenylformamidine (UV-1). The composition of the hindered amine light stabilizer and the ultraviolet absorber is the mixture (UV-3808) of 2,2,6,6-tetramethyl-4-piperidyl stearate (UV-3853) and hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate (UV2908).

[0032] In a preferred embodiment, the high melting point additive is an organic substance and / or an inorganic substance, and preferably, the high melting point additive is an additive for polymer materials. When an additive for polymer materials is used in a resin base material, better dispersibility and compatibility can be obtained, and even with a low usage amount, a better coating for the low melting point additive can be formed, and the anti-agglomeration performance of the masterbatch is improved. More preferably, the high melting point additive is an organic additive for polymer materials with a relative molecular mass greater than 500. When the above-mentioned organic additive for polymer materials is selected, in the manufacturing process of the masterbatch, it will precipitate from the surface of the masterbatch together with the melted low melting point additive in the granulation process. In addition, in the present application, such precipitation performance of the high melting point additive is also utilized. By sufficiently precipitating the high melting point additive in the granulation process of the masterbatch manufacturing process, in the subsequent cooling process, it will aggregate more sufficiently and be coated around the low melting point additive precipitated around it, so as to further suppress agglomeration after the masterbatch is formed. Using a high melting point additive with a relative molecular mass greater than 500 has a better promoting effect in preventing adhesion and agglomeration of the final masterbatch product. More preferably, the high melting point additive is an organic additive for polymer materials with a relative molecular mass greater than 600.

[0033] In a preferred embodiment, the high melting point additive is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite (Antioxidant 168, melting point 183-187 °C), 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (Antioxidant 3114, melting point 218-223 °C), 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene (Antioxidant 330, melting point 240-245 °C), and polyethylene wax (melting point 90-120 °C). These high melting point additives can not only better exert the precipitation and coating effects, but also, when forming a masterbatch together with the above low melting point additives, do not affect the subsequent use of the masterbatch and can also exert a better anti-degradation function. In particular, using Antioxidant 168, Antioxidant 330, and Antioxidant 3114, which are functional additives, not only plays a role in preventing the precipitation of the low melting point additive, but also has an anti-degradation effect when used in a resin substrate. Further, even if the above high melting point additives are not added in a very high ratio, the problem of agglomeration of the masterbatch can be effectively solved.

[0034] The resin substrate described in the present application may be adjusted according to the use environment of the additive masterbatch. For example, when adding the additive masterbatch to a polypropylene resin system, polypropylene resin may be selected as the resin substrate, and when adding the additive masterbatch to a polyethylene resin system, polyethylene resin may be selected as the resin substrate. Preferably, the resin substrate is a thermoplastic resin. The thermoplastic resin can directly become a component of a plastic product when processed later (even if it is different from the components of the product, since the addition amount of the additive masterbatch is generally small, it does not affect the performance of the plastic product), and can function as a better initial barrier layer against the melted low melting point additive.

[0035] More preferably, the resin substrate is a thermoplastic resin, and even more preferably, the thermoplastic resin is selected from one or more of polyolefin, polyester, polyether, polyketone, polyamide, polyurethane, polystyrene, high-impact polystyrene, polyacrylate, polymethacrylate, polyacetal, polyacrylonitrile, polybutadiene, acrylonitrile-butadiene-styrene copolymer, acrylonitrile-styrene copolymer, acrylate-styrene-acrylonitrile copolymer, cellulose acetate butyrate, cellulose polymer, polyimide, polyamideimide, polyetherimide, polyphenylene sulfide, polyphenylene ether, polysulfone, polyethersulfone, polyvinyl chloride, polycarbonate, poly(oxymethylene), ethylene-vinyl acetate copolymer.

[0036] More preferably, the resin substrate is a polyolefin. When polyolefin is adopted as the resin substrate, its versatility is higher, and when compounded with the above high melting point additive, the overall performance of the masterbatch can be improved better. Even more preferably, the polyolefin is selected from polypropylene and / or polyethylene.

[0037] In a preferred embodiment, based on parts by weight, the raw materials of the additive masterbatch include 30 to 70 parts of a resin base material (for example, it may be 30 parts, 32 parts, 35 parts, 40 parts, 42 parts, 44 parts, 45 parts, 46 parts, 48 parts, 50 parts, 52 parts, 55 parts, 58 parts, 60 parts, 65 parts, 70 parts), 0.1 to 30 parts of a high melting point additive (for example, it may be 0.1 part, 0.2 part, 0.5 part, 0.8 part, 1 part, 2 parts, 3 parts, 5 parts, 6 parts, 8 parts, 10 parts, 12 parts, 15 parts, 16 parts, 18 parts, 20 parts, 24 parts, 28 parts, 30 parts), and 30 to 70 parts of a low melting point additive (for example, it may be 30 parts, 32 parts, 35 parts, 40 parts, 42 parts, 44 parts, 45 parts, 46 parts, 48 parts, 50 parts, 52 parts, 55 parts, 58 parts, 60 parts, 65 parts, 70 parts). More preferably, based on parts by weight, the raw materials of the additive masterbatch include 30 to 70 parts of a resin base material, 1 to 25 parts of a high melting point additive, and 30 to 70 parts of a low melting point additive. Even more preferably, based on parts by weight, the raw materials of the additive masterbatch for polymer materials include 40 to 60 parts of a resin base material, 1 to 20 parts of a high melting point additive, and 40 to 60 parts of a low melting point additive. Even more preferably, the weight ratio of the high melting point additive to the low melting point additive is 1:3 to 15, and most preferably, it is 1:5 to 15. Limiting the usage amount of each component within the above range can effectively suppress problems such as agglomeration, and at the same time, the addition amount of the low melting point additive can be increased as much as possible.

[0038] In a preferred embodiment, the low melting point additive is one or more of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, a mixture of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate and hexadecyl 3,5 - di - tert - butyl - 4 - hydroxybenzoate, the resin base material is polyethylene or polypropylene, and the high melting point additive is one or more of tris(2,4 - di - tert - butylphenyl) phosphite (antioxidant 168), 1,3,5 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) - 1,3,5 - triazine - 2,4,6(1H,3H,5H) - trione (antioxidant 3114), 1,3,5 - trimethyl - 2,4,6 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) benzene (antioxidant 330), and polyethylene wax. The masterbatch formed by blending the high melting point additive, the low melting point additive, and the resin base material in the above - mentioned manner has better anti - sticking and agglomeration - preventing performance, and moreover, the anti - degradation performance of the additive itself is also better exerted.

[0039] Exemplarily, the additive masterbatch is 1 - 20 parts of tris(2,4 - di - tert - butylphenyl) phosphite, 30 - 50 parts of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, 30 - 50 parts of polypropylene resin, or 1 - 20 parts of 1,3,5 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) - 1,3,5 - triazine - 2,4,6(1H,3H,5H) - trione, 30 - 50 parts of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, 30 - 50 parts of polypropylene resin, or 1 - 20 parts of 1,3,5 - trimethyl - 2,4,6 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) benzene, 30 - 50 parts of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, 30 - 50 parts of polypropylene resin, or 0.1 to 10 parts of tris(2,4-di-tert-butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 0.1 to 10 parts of tris(2,4-di-tert-butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 0.1 to 10 parts of polyethylene wax, 0.1 to 10 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione and / or tris(2,4-di-tert-butylphenyl) phosphite and / or 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin.

[0040] As described above, the granulation process of the masterbatch in this application preferably adopts the usual method in this field. For example, the additive masterbatch is formed by performing screw extrusion, granulation, drying, and cooling on the raw materials in this order. Preferably, underwater cutting granulation is adopted for granulation, and the operating temperature is 190 to 230 °C.

[0041] The particle size of the additive masterbatch for the polymer material of this application may be adjusted according to needs. Preferably, the particle diameter is 1 to 5 mm.

[0042] In addition, the present application provides the use of the above-mentioned additive masterbatch in polymer materials. Since the additive masterbatch has excellent anti-agglomeration performance, it is also helpful for the dispersibility and compatibility of the masterbatch in the processing process of polymer materials. Specifically, the base material of the polymer material includes, but is not limited to, polyolefin, polyvinyl chloride, polyacetal, polyamide, styrene-based polymer, polyurethane, ABS resin, etc. Specific polymer material products include, but are not limited to, plastic products, thermoplastic elastomer products, rubber products, paints, adhesives, etc.

[0043] In short, the present application has the following advantages in terms of product quality and appearance compared with others, with a simple operation process, a wide range of applicable equipment, and stable production.

[0044] (1) The additive masterbatch of the present application has a high melting point additive as a protective layer, and the produced additive masterbatch does not show any agglomeration phenomenon even in a storage and transportation environment with high temperature or alternating high and low temperatures.

[0045] (2) The additive masterbatch of the present application has a simple manufacturing process, is easy for industrial batch production, has high stability, and does not affect the processing of downstream materials.

[0046] (3) Products with large and small particles can be manufactured according to the present application. In a fluidity ranking test where 500 g of weights are placed in a 50 °C beaker for 24 hours, the agglomeration fluidity of the additive masterbatch of the present application is ranked 1-2 in all cases, meeting the needs of diversification of downstream material processing.

[0047] Hereinafter, the present application will be described in more detail with specific examples. These examples should not be construed as limiting the scope of protection claimed in the present application.

[0048] (Example 1) In this example, a loss-in-weight type automatic weighing machine was used. PP resin and antioxidant 168 were added to a twin-screw extruder at the ratios described in Table 1 below. UV-3853 liquid was added to the twin-screw extruder using a liquid metering pump. After screw extrusion (for the extrusion process, refer to Table 2), underwater cutting, drying, and cooling were carried out to obtain a masterbatch with a particle size of 3.5 - 5 mm.

[0049]

Table 1

[0050]

Table 2

[0051] For the masterbatch product, a fluidity ranking test was carried out for 24 hours by putting 500 g of weights into a 50 °C beaker. The results are shown in the following table. For the photos before and after the test, refer to Figure 3 respectively, where (a) is the photo before the test and (b) is the photo after the test.

[0052] (Example 2) The difference between this example and Example 1 was only as follows. The component ratios are shown in Table 3. A small-diameter die was adopted in the extrusion process (for the extrusion process, refer to Table 4), and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0053]

Table 3

[0054]

Table 4

[0055] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass into a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 4 respectively, where (a) is the photo before the test and (b) is the photo after the test.

[0056] (Example 3) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 5, the extrusion process is shown in Table 6, and the particle size of the produced masterbatch was 3.5 - 5 mm.

[0057] [Table 5]

[0058] [Table 6]

[0059] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass into a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 5 respectively, where (a) is the photo before the test and (b) is the photo after the test.

[0060] (Example 4) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 7, the extrusion process is shown in Table 8, and the particle size of the produced masterbatch was 3.5 - 5 mm.

[0061] [Table 7]

[0062] [Table 8]

[0063] For the masterbatch product, a fluidity ranking test was conducted for 24 hours by putting 500 g of brass in a beaker at 50°C. The results are shown in the following table. For the photos before and after the test, refer to Figure 6 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0064] (Example 5) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 9, the extrusion process is shown in Table 10, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0065]

Table 9

[0066]

Table 10

[0067] For the masterbatch product, a fluidity ranking test was conducted for 24 hours by putting 500 g of brass in a beaker at 50°C. The results are shown in the following table. For the photos before and after the test, refer to Figure 7 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0068] (Example 6) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 11, the extrusion process is shown in Table 12, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0069]

Table 11

[0070]

Table 12

[0071] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass in a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 8 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0072] (Example 7) The difference between this example and Example 1 was only as follows. Refer to Table 13 for the component ratio, refer to Table 14 for the extrusion process, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0073] [Table 13]

[0074] [Table 14]

[0075] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass in a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 9 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0076] (Example 8) The difference between this example and Example 1 was only as follows. Refer to Table 15 for the component ratio, refer to Table 16 for the extrusion process, and the particle size of the produced masterbatch was 3.5 - 5 mm.

[0077] [Table 15]

[0078] [Table 16]

[0079] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of electrolytic copper into a beaker at 50°C for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 10 respectively, where (a) is the photo before the test and (b) is the photo after the test.

[0080] (Example 9) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 17, the extrusion process is shown in Table 18, and the particle size of the produced masterbatch was 3.5 - 5 mm.

[0081] [Table 17]

[0082] [Table 18]

[0083] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of electrolytic copper into a beaker at 50°C for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 11 respectively, where (a) is the photo before the test and (b) is the photo after the test.

[0084] (Example 10) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 19, the extrusion process is shown in Table 20, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0085] [Table 19]

[0086] [Table 20]

[0087] For the masterbatch product, a fluidity ranking test was conducted for 24 hours by putting 500 g of brass into a 50 °C beaker. Refer to the following table for the results. For the photos before and after the test, refer to Figure 12 respectively. Here, (a) is the photo before the test, and (b) is the photo after the test.

[0088] (Example 11) The difference between this example and Example 1 was only as follows. Refer to Table 21 for the component ratio, refer to Table 22 for the extrusion process, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0089]

Table 21

[0090]

Table 22

[0091] For the masterbatch product, a fluidity ranking test was conducted for 24 hours by putting 500 g of brass into a 50 °C beaker. Refer to the following table for the results. For the photos before and after the test, refer to Figure 13 respectively. Here, (a) is the photo before the test, and (b) is the photo after the test.

[0092] (Example 12) The difference between this example and Example 1 was only as follows. Refer to Table 23 for the component ratio, refer to Table 24 for the extrusion process, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0093]

Table 23

[0094]

Table 24

[0095] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass in a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 14 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0096] (Example 13) The difference between this example and Example 1 was only as follows. The component ratio is shown in Table 25, the extrusion process is shown in Table 26, and the particle size of the produced masterbatch was 1.0 - 2.5 mm.

[0097]

Table 25

[0098]

Table 26

[0099] For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass in a 50 °C beaker for 24 hours. The results are shown in the following table. For the photos before and after the test, refer to Figure 15 respectively. Here, (a) is the photo before the test and (b) is the photo after the test.

[0100] (Comparative Example 1) PP masterbatch product 1 (UV - 3853 weight content 50%) using a commercially available UV - 3853. For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of brass in a 50 °C beaker for 24 hours. The photo is shown in Figure 16.

[0101] The said product uses co - extrusion technology to form a protective material layer on the surface of a normal masterbatch product. However, when cutting with a cutter, the cut surface is not protected by the protective material, and moreover, the color is very dark yellow, and there is still an agglomeration phenomenon.

[0102] (Comparative Example 2) PP masterbatch product 2 (UV-3853 weight content 50%) using commercially available UV-3853, the fluidity of the product manufactured by foaming was ranked 4. For the masterbatch product, a fluidity ranking test was conducted by putting 500 g of weights into a beaker at 50 °C for 24 hours. The photo is shown in Fig. 17, and there were serious agglomerations.

[0103] (Comparative Example 3) The product (UV-3853 weight content 50%) manufactured according to the method described in CN113462079A, and the following was found in the production process. Since the raw materials were dilute, the melt pressure was low, and it was difficult to form a pressure difference during pelletizing. It was guaranteed that the particles were almost normal in the first 5 minutes, but later, flaky particles appeared and there was serious tailing. Moreover, since the raw materials were dilute, it was easy to vent up and clog the die, so the utilization rate of the raw materials was low and the product yield was low. Photos of the product at the beginning of production, the product after 5 minutes of production, and the product after the test are shown in Fig. 18. Here, Fig. (a) is the product at the beginning of production, Fig. (b) is the product after 5 minutes of production, and Fig. (c) is the photo of the product before the test.

[0104] The product manufactured with this formulation does not agglomerate, but the fluidity of the raw materials is close to the state after the melting of pure wax. The masterbatch has no strength with a very low resin content, has serious tailing, poor regularity, low density, is difficult to process, has poor equipment compatibility, and it is very difficult to produce stable batches. Also, during the process of processing and using this masterbatch, there is a risk that the strength is very low and the product will crack. Due to the characteristics of the raw materials, it is not possible to manufacture small-particle products in this process.

[0105] For the masterbatches manufactured in the above examples and comparative examples, the appearance was observed and the yield (qualified product quantity / input quantity) was calculated. The results are shown in Table 27.

[0106] The master batch products of the above examples and comparative examples were subjected to a fluidity ranking test in which a 500 g weight was placed in a beaker at 50° C. for 24 hours. The specific procedure was as follows.

[0107] 1. 50 g of the master batch was placed in a beaker, a can (made of a stainless steel disk) was placed on top of the powder or particles, and a 500 g weight was placed on top of the can.

[0108] 2. The beaker was placed in a forced air oven at 50°C for 24 hours (use a new sample for each temperature exposure).

[0109] 3. After taking out, the mixture was cooled to room temperature and kept for 2 hours.

[0110] 4. The following ranking criteria were applied to rank the samples for agglomeration, clogging, brittleness and flowability.

[0111] Rank 1: Free-flowing Rank 2: Some parts are lumpy and easily breakable (brittle) Rank 3: Mostly lumpy, can be broken down with a little force (relatively fragile) Rank 4: Most of the material is in a lump that does not disintegrate. Rank 5: Molten solid The results are shown in Table 27.

[0112] [Table 27]

[0113] As can be seen from the above results, the low melting point additive masterbatch prepared in the present application has excellent anti-agglomeration effect, and when baked in a forced air oven at 50°C for 24 hours, no sticking or agglomeration phenomenon was observed.

[0114] Moreover, the additive masterbatch of the present application has a simple production method, a stable process, a high output, a wide range of applicable equipment, a low cost, and moreover, there is no risk in use for downstream customers, and it has extremely high market competitiveness in both domestic and overseas markets.

[0115] The above are only preferred embodiments of the present application and do not limit the present application. Those skilled in the art can make various changes and modifications to the present application. Any changes, equivalent substitutions, improvements, etc. made within the spirit and scope of the present application shall all be included in the protection scope of the present application.

Claims

Claim 1 An additive masterbatch, the raw materials of which include a resin base material, a high melting point additive, and a low melting point additive, wherein the melting point of the high melting point additive is greater than 40°C, and the melting point of the low melting point additive is 40°C or less. The additive masterbatch is characterized by this. Claim 2 The low melting point additive is liquid or paste at room temperature, or a solid with a melting point of 40°C or less. Preferably, the melting point of the high melting point additive is greater than 80°C, more preferably greater than 100°C, still more preferably greater than 150°C, and even more preferably greater than 200°C. The additive masterbatch according to Claim 1 is characterized by this. Claim 3 The low melting point additive is a weather-resistant additive with a melting point of 40°C or less, preferably a light stabilizer with a melting point of 40°C or less. Preferably, the light stabilizer is a hindered amine light stabilizer and / or an ultraviolet absorber. More preferably, the additive masterbatch according to Claim 1 or 2 is characterized by being the hindered amine light stabilizer or a composition thereof. Claim 4 The hindered amine light stabilizer or a composition thereof is one or more selected from the reaction product of sebacic acid bis(2,2,6,6-tetramethyl-4-piperidyl) with tert-butyl hydroperoxide and octane, 2,2,6,6-tetramethyl-4-piperidyl stearate, the mixture of sebacic acid bis(1,2,2,6,6-pentamethyl-4-piperidyl) and sebacic acid mono(1,2,2,6,6-pentamethyl-4-piperidyl), bis(2,2,6,6-tetramethyl-1-undecyloxy-4-yl)-carbonate, and the mixture of 2,2,6,6-tetramethyl-4-piperidyl stearate and hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate. The additive masterbatch according to Claim 3 is characterized by this. Claim 5 The ultraviolet absorber is selected from one or more of benzotriazole-based ultraviolet absorbers, cyanoacrylate-based ultraviolet absorbers, benzamidine-based ultraviolet absorbers, benzophenone-based ultraviolet absorbers, hydroxyphenyltriazine-based ultraviolet absorbers, oxalic acid anilide-based ultraviolet absorbers, or salicylate-based ultraviolet absorbers. More preferably, the ultraviolet absorber is a reaction product of methyl 3-[3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyphenyl]propionate and PEG300, hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate, 2-ethylhexyl 2-cyano-3,3-diphenylacrylate, N-(ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine, and is selected from one or more of these. The additive masterbatch according to claim 3 is characterized by this.

6. The high melting point additive is an organic substance and / or an inorganic substance. Preferably, the high melting point additive is an additive for polymer materials. More preferably, the high melting point additive is an organic additive for polymer materials with a relative molecular mass greater than 500. Even more preferably, it is an organic additive for polymer materials with a relative molecular mass greater than 600. Even more preferably, the high melting point additive is selected from one or more of tris(2,4-di-tert-butylphenyl) phosphite, 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, polyethylene wax. Preferably, the resin base material is a thermoplastic resin, more preferably, the thermoplastic resin is selected from one or more of polyolefin, polyester, polyether, polyketone, polyamide, polyurethane, polystyrene, high impact polystyrene, polyacrylate, polymethacrylate, polyacetal, polyacrylonitrile, polybutadiene, acrylonitrile-butadiene-styrene copolymer, acrylonitrile-styrene copolymer, acrylate-styrene-acrylonitrile copolymer, cellulose acetate butyrate, cellulose polymer, polyimide, polyamideimide, polyetherimide, polyphenylene sulfide, polyphenylene ether, polysulfone, polyether sulfone, polyvinyl chloride, polycarbonate, poly(oxymethylene), ethylene vinyl acetate copolymer, More preferably, the resin base material is the polyolefin, still more preferably, the polyolefin is selected from polypropylene and / or polyethylene, The additive masterbatch according to any one of claims 1 to 4, characterized in that.

7. Based on parts by weight, the raw materials of the additive masterbatch include 30 to 70 parts of the resin base material, 0.1 to 30 parts of the high melting point additive, and 30 to 70 parts of the low melting point additive, More preferably, based on parts by weight, the raw materials of the additive masterbatch include 30 to 70 parts of the resin base material, 1 to 25 parts of the high melting point additive, and 30 to 70 parts of the low melting point additive, Still more preferably, based on parts by weight, the raw materials of the additive masterbatch include 40 to 60 parts of the resin base material, 1 to 20 parts of the high melting point additive, and 40 to 60 parts of the low melting point additive, Still more preferably, the weight ratio of the high melting point additive to the low melting point additive is 1:3 to 15, and most preferably 1:5 to 15, The additive masterbatch according to any one of claims 1 to 6, characterized in that.

8. The low melting point additive is one or more of 2,2,6,6-tetramethyl-4-piperidinyl stearate and a mixture of 2,2,6,6-tetramethyl-4-piperidinyl stearate and hexadecyl 3,5-di-tert-butyl-4-hydroxybenzoate, the resin base material is polyethylene or polypropylene, and the high melting point additive is one or more of tris(2,4-di-tert-butylphenyl) phosphite, 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, and polyethylene wax, Preferably, the additive masterbatch is, 1 to 20 parts of tris(2,4-di-tert-butylphenyl) phosphite, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 20 parts of 1,3,5-tris(3,5-di-tert-butyl-4-hydroxybenzyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 20 parts of 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 10 parts of tris(2,4-di-tert-butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6-tetramethyl-4-piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 10 parts of tris(2,4 - di - tert - butylphenyl) phosphite, 0.1 to 10 parts of 1,3,5 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) - 1,3,5 - triazine - 2,4,6(1H,3H,5H) - trione, 30 to 50 parts of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, 30 to 50 parts of polypropylene resin, or 1 to 10 parts of polyethylene wax, 0.1 to 10 parts of 1,3,5 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl) - 1,3,5 - triazine - 2,4,6(1H,3H,5H) - trione and / or tris(2,4 - di - tert - butylphenyl) phosphite and / or 1,3,5 - trimethyl - 2,4,6 - tris(3,5 - di - tert - butyl - 4 - hydroxybenzyl)benzene, 30 to 50 parts of 2,2,6,6 - tetramethyl - 4 - piperidinyl stearate, 30 to 50 parts of polypropylene resin, characterized in that it comprises an additive masterbatch according to any one of claims 1 to 7.

9. The additive masterbatch is formed by performing screw extrusion, granulation, drying, and cooling on the raw materials in this order. Preferably, underwater pelletizing is employed for the granulation, and the operating temperature is 190 to 230 °C. Preferably, the particle size of the additive masterbatch for the polymer material is 1 to 5 mm, characterized in that it is an additive masterbatch according to any one of claims 1 to 9.

10. Use of the additive masterbatch according to any one of claims 1 to 9 in a polymer material.

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