Compatilizer, composite material, preparation method of composite material and electronic cigarette tar cup

Abstract

The invention provides a compatilizer, a composite material, a preparation method of the composite material and an electronic cigarette liquid cup, and belongs to the technical field of electronic cigarette application. The compatilizer disclosed by the invention is prepared from an ethylene-acrylic acid copolymer, a maleic anhydride grafted ethylene-octylene copolymer, beta-(3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecanol propionate and tert-butyl cumene peroxide which are subjected to melt mixing. The invention also provides a PCTG-PP5 composite material adopting the compatilizer and a preparation method thereof, and the PCTG-PP5 composite material is applied to raw material injection molding of an electronic cigarette liquid cup, so that the processed electronic cigarette liquid cup simultaneously has the advantages of PCTG and PP5 materials, various properties can meet the requirements of the electronic cigarette liquid cup, and the product cost is remarkably reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of electronic cigarette applications, and in particular to a PCTG-PP5 composite material for an electronic cigarette oil cup and a preparation method thereof, and also to a compatibilizer used for processing the PCTG-PP5 composite material. Background Art

[0002] With the rapid development of the e-cigarette industry, e-cigarette oil cups, as one of its core components, have placed higher demands on material performance and price. Traditional e-cigarette oil cups are mostly made of single materials such as PCTG (polyethylene terephthalate-1,4-cyclohexanedimethanol), PP (polypropylene), or PC (polycarbonate), but these materials have limitations in certain aspects. For example, while PCTG offers excellent transparency and chemical resistance, it is relatively expensive. While PP5 offers lower cost and good heat resistance, its transparency, impact strength, and flame retardancy are relatively poor. Therefore, the development of a composite material that combines the advantages of PCTG and PP5 has become an urgent need for industry development.

[0003] However, the solubility parameter of PCTG is 20.025 (J / cm 3 ) 1 / 2 , the solubility parameter of PP5 is 16.3 (J / cm 3 ) 1 / 2 The solubility parameters of the two differ by 3.7 (J / cm³)¹ / 2, making them thermodynamically incompatible. Furthermore, PCTG has a linear thermal expansion coefficient of 1×10⁻⁵ to 2×10⁻⁵ K⁻⁵, and a molding shrinkage of 0.2% to 0.3%. PP5 has a linear thermal expansion coefficient of approximately 11×10⁻⁵ K⁻⁵, and a molding shrinkage of 0.7% to 1.4%. These significant differences in properties lead to significant incompatibility when blending the two, resulting in the resulting composite material failing to meet the excellent heat resistance, chemical resistance, flame retardancy, and mechanical strength requirements of the oil cup. Summary of the Invention

[0004] In order to solve the problems in the prior art, the present invention provides a compatibilizer, which can achieve good compatibility between PCTG and PP5 under its connecting effect. It also provides a PCTG-PP5 composite material using the compatibilizer and a preparation method thereof, and applies the compatibilizer to the raw material injection molding of an electronic cigarette oil cup, so that the processed electronic cigarette oil cup has the advantages of both PCTG and PP5 materials, and all performances can meet the requirements of the electronic cigarette oil cup, and significantly reduces the product cost.

[0005] The compatibilizer of the present invention comprises melt-mixed ethylene-acrylic acid copolymer, maleic anhydride grafted ethylene-octene copolymer, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide, wherein the mass ratio of the ethylene-acrylic acid copolymer, maleic anhydride grafted ethylene-octene copolymer, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide is 0.5-2:0.5-2:0.005-0.02:0.02-0.08.

[0006] Furthermore, the mass ratio of the ethylene-acrylic acid copolymer, the maleic anhydride grafted ethylene-octene copolymer, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide is 1:1:0.01:0.05.

[0007] The present invention also provides a PCTG-PP5 composite material, comprising the above-mentioned compatibilizer and the following components in parts by weight:

[0008]

[0009] The weight content of the compatibilizer in the PCTG-PP5 composite material is 3 to 10 parts.

[0010] Furthermore, the toughening agent is at least one of glycidyl methacrylate grafted ethylene-octene random copolymer, POE toughening agent, SEBS maleic anhydride grafted, and EPDM rubber.

[0011] Furthermore, the antioxidant includes at least one of type 1010 antioxidant, type 1098 antioxidant, type 168 antioxidant, and type 626 antioxidant.

[0012] Furthermore, the silane coupling agent includes at least one of KH550, KH560, KH570, and KH602.

[0013] Furthermore, the lubricant includes at least one of stearate, fatty acid, fatty acid amide, and organosilicon compound.

[0014] Furthermore, the antibacterial agent includes at least one of sorbitol, benzoic acid and its sodium salt, sodium propionate, and propionic acid.

[0015] The present invention also provides a method for preparing a PCTG-PP5 composite material, which is used to prepare the PCTG-PP5 composite material, comprising the following steps:

[0016] S1: drying PP5 in a vacuum oven at a first temperature for a first set time, and drying PCTG in a vacuum oven at a second temperature for a second set time;

[0017] S2: PP5, PCTG, compatibilizer, toughening agent, antioxidant, silane coupling agent, lubricant and antibacterial agent are uniformly mixed in a certain proportion and fed into a twin-screw melt extruder for processing;

[0018] S3: The extrudate in step S2 is cooled, and then pelletized by a pelletizer to obtain a PCTG-PP5 composite material.

[0019] The present invention also provides an electronic cigarette oil cup, which is made by injection molding using the PCTG-PP5 composite material.

[0020] Compared with the prior art, the beneficial effect of the present invention is that the synergistic cooperation of the various components of the compatibilizer of the present invention enables the present invention to form a new type of acrylic compatibilizer whose main chain segment is compatible with PCTG and whose side chain segment is compatible with PP5, thereby improving the compatibility of PCTG and PP5, so that the prepared electronic cigarette oil cup meets the required requirements of good heat resistance, good chemical resistance, flame retardancy and mechanical strength. DETAILED DESCRIPTION

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meanings as commonly understood by those skilled in the art to which the present invention belongs. The terms used in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The terms "including" and "having" and any variations thereof in the specification and claims of the present invention are intended to cover non-exclusive inclusions. The terms "first" and "second" in the specification and claims of the present invention are used to distinguish different objects, not to describe a specific order.

[0022] References to "embodiments" in this disclosure mean that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the disclosure. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor does it necessarily refer to mutually exclusive, independent, or alternative embodiments to other embodiments. It is understood, both explicitly and implicitly, by those skilled in the art that the embodiments described in this disclosure may be combined with other embodiments.

[0023] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions of the present invention will be clearly and completely described below in conjunction with embodiments.

[0024] The invention provides a compatibilizer, which is characterized by comprising melt-mixed ethylene-acrylic acid copolymer, maleic anhydride grafted ethylene-octene copolymer, beta-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide.

[0025] The mass ratio of the ethylene-acrylic acid copolymer (EMA), maleic anhydride grafted ethylene-octene copolymer (MAH-g-PE, grafting rate 1.2%), β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide is 0.5-2:0.5-2:0.005-0.02:0.02-0.08. Preferably, the mass ratio of the ethylene-acrylic acid copolymer, maleic anhydride grafted ethylene-octene copolymer, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide in this example is 1:1:0.01:0.05.

[0026] The processing method of the compatibilizer of this example is as follows: according to the required mass ratio, a certain amount of raw materials are weighed, and then melt-blended, extruded and granulated to obtain the compatibilizer of the present invention.

[0027] The ethylene segments in the ethylene-acrylic acid copolymer of the present invention have excellent compatibility with the non-polar plastic PP, and can be physically entangled or dissolved in it. The acrylic acid segments in EMA provide highly reactive carboxylic acid groups. These groups, in a molten state and in the presence of an initiator, can react with the anhydride groups of the maleic anhydride-grafted ethylene-octene copolymer to form an EMA-MAH-g-PE copolymer or crosslinked network. The resulting esterified backbone segment is highly compatible with PCTG. Furthermore, the POE segments exhibit good compatibility with the non-polar plastic component PP5.

[0028] Due to the high temperature and high shear conditions of melt blending, the above-mentioned two compatibilizers themselves are very prone to oxidative degradation, producing alkyl free radicals. These free radicals can trigger a chain reaction, resulting in molecular chain breakage (degradation) or crosslinking, seriously deteriorating material properties. Therefore, this example, by increasing β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecanol ester 1076 type, as a hindered phenol antioxidant, its phenolic hydroxyl group can efficiently capture these alkyl free radicals, terminate the chain oxidation reaction, and the phenoloxy free radical generated is relatively stable and will not cause new degradation. Therefore, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecanol ester of the present invention can protect the molecular chains of EMA and MAH-g-PE from oxidative degradation during processing, ensure the integrity of its molecular weight and reactive groups, thereby ensuring their effectiveness in interfacial reactions.

[0029] The tert-butyl isopropyl benzene peroxide of the present invention serves as an initiator in the compatibilizer of the present invention. At the high temperature of melt blending, the tert-butyl isopropyl benzene peroxide decomposes to generate highly active free radicals (mainly tert-butyloxy free radicals and methylbenzyl free radicals). These free radicals are the core driving force of the entire reactive compatibilizing system, can initiate the grafting reaction of the two compatibilizers, and promote the interfacial reaction to generate a copolymer containing two reactive groups, thereby further enhancing the compatibilizing effect.

[0030] Therefore, the present invention, through the coordination of various components and the synergistic effect of physically compatible segments, highly active reactive groups, free radical initiators and antioxidants, in situ constructs a strong "chemical-physical" bridge at the interface of the incompatible two phases, thereby achieving good compatibility between the originally incompatible PCTG and PP5 materials.

[0031] The present invention also provides a PCTG-PP5 composite material, comprising the following components in parts by weight:

[0032]

[0033] Preferably, the toughening agent in this example is at least one of glycidyl methacrylate grafted ethylene-octene random copolymer, POE toughening agent, SEBS grafted maleic anhydride, and EPDM rubber.

[0034] The antioxidant in this example includes at least one of type 1010 antioxidant, type 1098 antioxidant, type 168 antioxidant, and type 626 antioxidant.

[0035] The silane coupling agent in this example can be selected from at least one or all of KH550, KH560, KH570, and KH602. The lubricant in this example includes at least one of stearate, fatty acid, fatty acid amide, and organosilicon compound. The antibacterial agent in this example includes at least one of sorbitol, benzoic acid and its sodium salt, sodium propionate, and propionic acid.

[0036] The preparation method of the PCTG-PP5 composite material of the present invention is:

[0037] S1: drying PP5 in a vacuum oven at a first temperature for a first set time, and drying PCTG in a vacuum oven at a second temperature for a second set time;

[0038] S2: PP5, PCTG, compatibilizer, toughening agent, antioxidant, silane coupling agent, lubricant and antibacterial agent are uniformly mixed in a certain proportion and fed into a twin-screw melt extruder for processing;

[0039] S3: The extrudate in step S2 is cooled, and then pelletized by a pelletizer to obtain a PCTG-PP5 composite material.

[0040] The electronic cigarette oil cup of the present invention is made by injection molding using the PCTG-PP5 composite material.

[0041] Preferably, in step S2, the extrusion temperature is 220-240°C, the rotation speed during the melting process is 200-300 r / min, and the mixing rotation speed is 1000-4000 r / min.

[0042] The PCTG-PP5 composite material of the present invention has the following advantages:

[0043] 1. Improve product performance: Through the compounding of PCTG and PP5, the chemical resistance, impact resistance and flame retardancy of PCTG are retained, and its temperature resistance is improved, so that the composite material shows better performance in the electronic cigarette oil cup.

[0044] 2. Reduce costs: PP5 has a low cost. After compounding with PCTG, it can reduce costs while maintaining high performance and improve the market competitiveness of the product.

[0045] 3. Environmental protection: PCTG and PP5 are both environmentally friendly materials. The composite products meet environmental protection requirements and are suitable for food contact and medical fields.

[0046] 4. Easy to process: The addition of PP5 reduces the melt viscosity of PCTG and improves the processability of the product. It is suitable for injection molding, blow molding, hot pressing and other molding processes, and is convenient for large-scale production.

[0047] The effects of the present invention are demonstrated below through specific examples and experimental data. The compatibilizer in this example is referred to as compatibilizer A. The contents of the various components of the electronic cigarette liquid cups of Examples 1-12 are shown in Tables 1 and 2.

[0048] Table 1 Content of each component in Examples 1-6

[0049] Components Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 PCTG 20 40 15 30 20 20 PP5 60 40 65 50 60 60 Compatibilizer A 10 8 10 10 8 9 Toughening agent POE-g-GMA 3 3 3 3 5 4 Silane coupling agent KH560 5 7 5 5 5 5 1010 antioxidant 0.15 0.15 0.15 0.15 0.15 0.15 168 antioxidant 0.15 0.15 0.15 0.15 0.15 0.15 Lubricant fatty acid amide 1 1 1 1 1 1 Antibacterial agent sorbitol 0.7 0.7 0.7 0.7 0.7 0.7

[0050] Table 2 Content of each component in Examples 7-12

[0051]

[0052]

[0053] The preparation method of the electronic cigarette oil cup prepared by using the composite material of the present invention is as follows:

[0054] S1. Dry PP5 in a vacuum oven at 70°C for 4 h, and PCTG in a vacuum oven at 80°C for 12 h.

[0055] S2, PP5, PCTG, compatibilizer A, toughening agent, antioxidant, silane coupling agent, lubricant and antibacterial agent were uniformly mixed according to the weight ratio of the above embodiment, and fed into a twin-screw melt extruder for processing, wherein the extrusion temperature was 220 ° C, the speed during the melting process was 250 r / min, and the mixing speed was 2000 r / min;

[0056] S3, cooling the extrudate in step S2 with water, and pelletizing it with a pelletizer to obtain a PCTG-PP5 composite material;

[0057] S4: Add the PCTG-PP5 composite material into the e-cigarette oil cup injection molding machine, cool it to form and demold it, and finally obtain the finished e-cigarette oil cup.

[0058] Comparative Example 1

[0059] Comparative Example 1 provides a PCTG-PP5 composite material, which has the same formula, dosage and preparation method as Example 1, except that a single compatibilizer EMA is used instead of the specially prepared compatibilizer A of the present invention.

[0060] Comparative Example 2

[0061] Comparative Example 2 provides a PCTG-PP5 composite material, which has the same formula, dosage and preparation method as Example 1, except that a single compatibilizer, maleic anhydride grafted ethylene-octene copolymer (MAH-g-PE, grafting rate 1.2%), is used instead of the specially prepared compatibilizer A of the present invention.

[0062] Comparative Example 3

[0063] Comparative Example 3 provides a PCTG-PP5 composite material, which has the same formula, dosage and preparation method as Example 1, except that compatibilizer B is used instead of the specially prepared compatibilizer A of the present invention, and compatibilizer B is melt-mixed by ethylene-acrylic acid copolymer (EMA) and maleic anhydride grafted ethylene-octene copolymer (MAH-g-PE, grafting rate 1.2%) in a mass ratio of 1:1.

[0064] Comparative Example 4

[0065] Comparative Example 4 provides a PCTG-PP5 composite material with the same formulation, dosage, and preparation method as Example 1, except that compatibilizer C is used instead of the specially prepared compatibilizer A of the present invention. Compatibilizer C is composed of ethylene-acrylic acid copolymer (EMA), maleic anhydride-grafted ethylene-octene copolymer (MAH-g-PE, grafting ratio 1.2%), antioxidant β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate 1076, and initiator tert-butyl cumyl peroxide. The mixture is melt-blended and extruded into pellets in a mass ratio of 1:1:0.01:0.01.

[0066] Test results

[0067] The electronic cigarette oil cups prepared in Examples 1-12 and Comparative Examples 1-4 were subjected to chemical corrosion resistance test, ball drop test, flame retardancy test, high temperature and high humidity test, negative pressure test, low temperature storage test and hot and cold shock test, respectively. The test results are shown in Table 3.

[0068] Table 3 Test data of Examples 1-12 and Comparative Examples 1-4

[0069]

[0070] A comprehensive analysis of Example 1 and Comparative Examples 1-4 revealed that the e-cigarette e-cigarette cup prepared in Example 1 exhibited excellent heat resistance, chemical resistance, flame retardancy, and mechanical strength, demonstrating that the type of compatibilizer also has a certain impact on the performance of the composite material. Using the compatibilizer A synthesized by this invention, a novel acrylic compatibilizer with a main chain segment compatible with PCTG and a side chain segment compatible with PP5, developed through reactive extrusion based on the non-reactive compatibilizer EMA, not only fully compatibilizes the two individual materials but also effectively enhances the strength of the composite material at the weld line, ensuring that the composite material meets the performance requirements of an e-cigarette e-cigarette cup.

[0071] The specific implementation manner described above is a preferred implementation manner of the present invention, and is not intended to limit the specific implementation scope of the present invention. The scope of the present invention includes but is not limited to this specific implementation manner. All equivalent changes made in accordance with the present invention are within the protection scope of the present invention.

Claims

1. A compatibilizer, characterized in that: The invention comprises melt-blended ethylene-acrylic acid copolymer, maleic anhydride grafted ethylene-octene copolymer, beta-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide.

2. The compatibilizer according to claim 1, characterized in that: The mass ratio of the ethylene-acrylic acid copolymer, the maleic anhydride grafted ethylene-octene copolymer, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate and tert-butyl isopropyl benzene peroxide is 1:1:0.01:0.

05.

3. A PCTG-PP5 composite material comprising the compatibilizer according to claim 1 or 2, characterized in that: Also includes the following components by weight: The weight content of the compatibilizer in the PCTG-PP5 composite material is 3 to 10 parts.

4. The PCTG-PP5 composite material according to claim 3, characterized in that: The toughening agent is at least one of glycidyl methacrylate grafted ethylene-octene random copolymer POE-g-GMA, POE toughening agent, SEBS maleic anhydride grafted, and EPDM rubber.

5. The PCTG-PP5 composite material according to claim 1, characterized in that: The antioxidant includes at least one of 1010 type antioxidant, 1098 type antioxidant, 168 type antioxidant, and 626 type antioxidant.

6. The PCTG-PP5 composite material according to claim 1, characterized in that: The silane coupling agent includes at least one of KH550, KH560, KH570, and KH602.

7. The PCTG-PP5 composite material according to claim 1, characterized in that: The lubricant includes at least one of stearate, fatty acid, fatty acid amide, and organosilicon compound.

8. The PCTG-PP5 composite material according to claim 1, characterized in that: The antibacterial agent includes at least one of sorbitol, benzoic acid and its sodium salt, sodium propionate, and propionic acid.

9. A method for preparing a PCTG-PP5 composite material, for preparing the PCTG-PP5 composite material according to any one of claims 3 to 8, characterized in that: The steps include: S1: drying PP5 in a vacuum oven at a first temperature for a first set time, and drying PCTG in a vacuum oven at a second temperature for a second set time; S2: PP5, PCTG, compatibilizer, toughening agent, antioxidant, silane coupling agent, lubricant and antibacterial agent are uniformly mixed in a certain proportion and fed into a twin-screw melt extruder for processing; S3: The extrudate in step S2 is cooled, and then pelletized by a pelletizer to obtain a PCTG-PP5 composite material.

10. An electronic cigarette oil cup, characterized by: The PCTG-PP5 composite material according to any one of claims 3 to 8 is produced by injection molding.

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