A composite flame-retardant nylon 6 material and its preparation method

Abstract

This invention relates to the field of nylon 6 technology, and more particularly to a composite flame-retardant nylon 6 material and its preparation method. The raw materials of the aforementioned composite flame-retardant nylon 6 material, by weight, include: 70-100 parts nylon 6, 10-20 parts activated polyphenylene sulfide chopped fibers, 5-15 parts environmentally friendly flame retardant, 1-3 parts flame retardant synergist, 1-5 parts SEBS-g-MAH, 1-5 parts acrylonitrile-styrene copolymer, 1-2 parts talc, 1-3 parts pentaerythritol phosphate, 1-3 parts nano-silica, 1-2 parts dodecyl stearic acid, 1-2 parts fatty amine polyoxyethylene ether, 1-3 parts lubricant, and 1-2 parts antioxidant. The environmentally friendly flame retardant raw materials include: DOPO flame retardant, vinyltriethoxysilane, and γ-glycidyl etheroxypropyltrimethoxysilane. This invention is halogen-free, significantly improves the flame retardant rating and smoke suppression and anti-dripping properties of the material, and effectively maintains the excellent mechanical properties of the composite material.

Description

Technical Field

[0001] This invention relates to the field of nylon 6 technology, and in particular to a composite flame-retardant nylon 6 material and its preparation method. Background Technology

[0002] Nylon, a polymer compound containing amide groups in its main chain, is an important engineering resin with wide applications in daily life and industry. Among them, PA6 (Nylon 6) is the most produced and widely used nylon variety due to its high mechanical strength, high melting point, wear resistance, oil resistance, and excellent heat resistance.

[0003] In many applications, especially in electronic and electrical components (such as terminals, sockets, and switch housings) and in areas where stringent fire safety standards need to be met, the flame-retardant properties of nylon itself are often insufficient to meet safety requirements.

[0004] Currently, the most common industrial approach to flame retardancy involves adding flame retardants, such as halogenated, phosphorus-based, nitrogen-based, and inorganic metal hydroxides, to the nylon matrix. However, this method has significant limitations: most flame retardants have poor compatibility with the highly polar nylon matrix, resulting in uneven dispersion and agglomeration. This not only affects the flame retardancy efficiency but also acts as stress defects, significantly deteriorating the material's mechanical properties, such as reducing impact strength and tensile strength.

[0005] Therefore, it is of great practical significance to find a flame-retardant nylon 6 material that can effectively improve the flame retardancy of nylon while maintaining its good mechanical properties. Summary of the Invention

[0006] The purpose of this invention is to address the shortcomings of existing technologies by proposing a composite flame-retardant nylon 6 material and its preparation method.

[0007] A composite flame-retardant nylon 6 material, the raw materials of which, by weight, include: 70-100 parts nylon 6, 10-20 parts activated polyphenylene sulfide chopped fibers, 5-15 parts environmentally friendly flame retardant, 1-3 parts flame retardant synergist, 1-5 parts SEBS-g-MAH, 1-5 parts acrylonitrile-styrene copolymer, 1-2 parts talc, 1-3 parts pentaerythritol phosphate, 1-3 parts nano silica, 1-2 parts dodecyl stearic acid, 1-2 parts fatty amine polyoxyethylene ether, 1-3 parts lubricant, and 1-2 parts antioxidant; the raw materials of the environmentally friendly flame retardant include: DOPO flame retardant, vinyltriethoxysilane, and γ-glycidoxypropyltrimethoxysilane.

[0008] Preferably, the activated polyphenylene sulfide chopped fiber is a silane coupling agent activated polyphenylene sulfide chopped fiber; specifically: 1-3 parts by weight of KH-550 coupling agent are added to 50-80 parts of a 50-60 wt% ethanol aqueous solution and stirred evenly, then 10-20 parts of polyphenylene sulfide chopped fiber are added, stirred at 50-60℃ for 10-20 minutes, filtered, washed with deionized water, and vacuum dried to obtain activated polyphenylene sulfide chopped fiber.

[0009] Preferably, the flame retardant synergist is zinc borate.

[0010] Preferably, the lubricant is ethylene bis-stearamide.

[0011] Preferably, the antioxidants include: antioxidant 1010 and antioxidant 168.

[0012] More preferably, the mass ratio of antioxidant 1010 to antioxidant 168 is 1-2:1.

[0013] Preferably, the mass ratio of DOPO flame retardant, vinyltriethoxysilane, and γ-glycidoxypropyltrimethoxysilane is 5-10:1-4:1-2.

[0014] Preferably, the environmentally friendly flame retardant is prepared by the following steps: DOPO flame retardant is added to anhydrous toluene and stirred evenly. Vinyltriethoxysilane and AIBN are added, and the mixture is heated to 80-90℃ and stirred for 2-6 hours under nitrogen protection. The solvent is removed, and the product and γ-glycidoxypropyltrimethoxysilane are added to an ethanol aqueous solution. Triethylamine is added to adjust the pH of the system to 8-8.5, and the mixture is stirred at 50-70℃ for 2-4 hours. The solvent is removed, and the mixture is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0015] More preferably, the mass fraction of the ethanol aqueous solution is 40-60%.

[0016] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly and extruding and granulating.

[0017] Preferably, a twin-screw extruder is used for extrusion granulation, with the temperatures in each zone of the twin-screw extruder being 200-205℃, 210-215℃, 220-230℃, 230-235℃, 230-235℃, and 230-235℃, respectively, and the screw speed being 60-100 r / min.

[0018] Compared with existing technologies, the present invention has the following advantages: The composite flame-retardant nylon 6 material obtained by this invention achieves enhanced flame retardancy while maintaining mechanical properties and environmental friendliness through the synergistic effect of various materials. Activated polyphenylene sulfide is added in fibrous form, utilizing its intrinsic flame retardancy and reinforcing effect to effectively compensate for mechanical properties while enhancing the flame retardant effect.

[0019] This invention, through the formation of an organic-inorganic hybrid structure in an environmentally friendly flame retardant, not only significantly improves compatibility with the nylon matrix and prevents agglomeration, but also effectively constructs a stable flame-retardant barrier during combustion, providing effective heat and oxygen insulation and inhibiting dripping. Furthermore, zinc borate acts as a synergist, further strengthening the flame-retardant barrier at high temperatures. The combined effect with nylon 6 avoids stress concentration and mechanical degradation caused by agglomeration points, ensuring that the flame-retardant components function efficiently and synergistically during combustion. This invention utilizes a combination of lubricants and antioxidants to ensure good processability and thermal stability.

[0020] This invention is not only halogen-free, which aligns with environmental protection trends, but also effectively maintains the excellent mechanical properties of composite materials while significantly improving their flame retardancy and smoke suppression and anti-dripping performance, achieving a balance in overall performance. Furthermore, the preparation method is simple and suitable for large-scale promotion and utilization. Attached Figure Description

[0021] Figure 1 The image shows a comparison of the tensile strength and flexural strength of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2.

[0022] Figure 2 The chart shows a comparison of the notched impact strength and oxygen index of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2. Detailed Implementation

[0023] The present invention will now be described in further detail with reference to specific embodiments. The given embodiments are merely illustrative of the invention and not intended to limit its scope. The embodiments provided below can serve as a guide for further improvements by those skilled in the art and do not constitute a limitation on the invention in any way.

[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0025] The nylon 6 used below is sourced from Sinopec Baling, model PA6 BL2280-Z. The SEBS-g-MAH used below is purchased from Guangdong Mouheng New Material Technology Co., Ltd., with a grafting rate of 1.0-2.0%. The acrylonitrile-styrene copolymer used below is sourced from PetroChina Jilin Petrochemical, grade SAN-2437.

[0026] The activated polyphenylene sulfide (PPS) chopped fibers used below are silane coupling agent-activated PPS chopped fibers. Specifically, 2g of KH-550 coupling agent is added to 60g of a 60wt% ethanol aqueous solution and stirred until homogeneous. Then, 15g of PPS chopped fibers are added, and the mixture is stirred at 55℃ for 15 minutes. After filtration, the fibers are washed with deionized water and vacuum dried to obtain activated PPS chopped fibers. The PPS chopped fibers used are sourced from Toray Industries, Japan, and are TORCON™ PPS fibers.

[0027] Example 1 A composite flame-retardant nylon 6 material, comprising the following raw materials: 70g nylon 6, 10g activated polyphenylene sulfide chopped fibers, 5g environmentally friendly flame retardant, 1g zinc borate, 1g SEBS-g-MAH, 1g acrylonitrile-styrene copolymer, 1g talc, 1g pentaerythritol phosphate, 1g nano-silica, 1g dodecyl stearic acid, 1g fatty amine polyoxyethylene ether, 1g ethylene bis-stearamide, and 1g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a 1:1 mass ratio.

[0028] The environmentally friendly flame retardant is prepared by the following steps: 5g of DOPO flame retardant is added to 40g of anhydrous toluene and stirred evenly. 1g of vinyltriethoxysilane and 0.01g of AIBN are added. Under nitrogen protection, the mixture is heated to 80℃ and stirred for 2h. The solvent is removed by vacuum distillation. The product and 1g of γ-glycidyl etheroxypropyltrimethoxysilane are added to 40g of a 50% (w / w) aqueous ethanol solution. Triethylamine is added to adjust the pH of the system to 8-8.5. The mixture is stirred at 50℃ for 2h. The solvent is removed by vacuum distillation. The product is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0029] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 200℃, 210℃, 220℃, 230℃, 230℃, 230℃, and 230℃, respectively, and the screw speed is 60 r / min.

[0030] Example 2 A composite flame-retardant nylon 6 material comprises the following raw materials: 100g nylon 6, 20g activated polyphenylene sulfide chopped fibers, 15g environmentally friendly flame retardant, 3g zinc borate, 5g SEBS-g-MAH, 5g acrylonitrile-styrene copolymer, 2g talc, 3g pentaerythritol phosphate, 3g nano-silica, 2g dodecyl stearic acid, 2g fatty amine polyoxyethylene ether, 3g ethylene bis-stearamide, and 2g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 2:1.

[0031] The environmentally friendly flame retardant is prepared by the following steps: 10g of DOPO flame retardant is added to 60g of anhydrous toluene and stirred evenly. 4g of vinyltriethoxysilane and 0.02g of AIBN are added. Under nitrogen protection, the mixture is heated to 90℃ and stirred for 6h. The solvent is removed by vacuum distillation. The product and 2g of γ-glycidyl etheroxypropyltrimethoxysilane are added to 60g of 60% ethanol aqueous solution. Triethylamine is added to adjust the pH of the system to 8-8.5. The mixture is stirred at 70℃ for 4h. The solvent is removed by vacuum distillation. The product is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0032] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 205℃, 215℃, 230℃, 235℃, 235℃, 235℃, and 235℃, respectively, and the screw speed is 70 r / min.

[0033] Example 3 A composite flame-retardant nylon 6 material comprises the following raw materials: 80g nylon 6, 18g activated polyphenylene sulfide chopped fibers, 8g environmentally friendly flame retardant, 2.5g zinc borate, 2g SEBS-g-MAH, 4g acrylonitrile-styrene copolymer, 1.2g talc, 2.5g pentaerythritol phosphate, 1.5g nano-silica, 1.8g dodecyl stearic acid, 1.3g fatty amine polyoxyethylene ether, 1.5g ethylene bis-stearamide, and 1.7g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 1.2:1.

[0034] The environmentally friendly flame retardant was prepared using the following steps: 6g of DOPO flame retardant was added to 45g of anhydrous toluene and stirred until homogeneous. 4g of vinyltriethoxysilane and 0.01g of AIBN were added, and the mixture was heated to 80℃ and stirred for 2 hours under nitrogen protection. The solvent was removed by vacuum distillation. The product and 1.5g of γ-glycidoxypropyltrimethoxysilane were added to 45g of a 45% (w / w) aqueous ethanol solution. Triethylamine was added to adjust the pH of the system to 8-8.5. The mixture was stirred at 55℃ for 3 hours, and the solvent was removed by vacuum distillation. The product was then pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0035] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 202℃, 212℃, 225℃, 233℃, 233℃, 232℃, and 232℃, respectively, and the screw speed is 100r / min.

[0036] Example 4 A composite flame-retardant nylon 6 material comprises the following raw materials: 90g nylon 6, 12g activated polyphenylene sulfide chopped fibers, 12g environmentally friendly flame retardant, 1.5g zinc borate, 4g SEBS-g-MAH, 2g acrylonitrile-styrene copolymer, 1.8g talc, 1.5g pentaerythritol phosphate, 2.5g nano-silica, 1.2g dodecyl stearic acid, 1.7g fatty amine polyoxyethylene ether, 2.5g ethylene bis-stearamide, and 1.3g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 1.8:1.

[0037] The environmentally friendly flame retardant was prepared using the following steps: 8g of DOPO flame retardant was added to 50g of anhydrous toluene and stirred until homogeneous. 3g of vinyltriethoxysilane and 0.02g of AIBN were added. Under nitrogen protection, the mixture was heated to 88℃ and stirred for 5 hours. The solvent was removed by vacuum distillation. The product and 1.5g of γ-glycidyl etheroxypropyltrimethoxysilane were added to 55g of a 58% (w / w) aqueous ethanol solution. Triethylamine was added to adjust the pH of the system to 8-8.5. The mixture was stirred at 60℃ for 3 hours. The solvent was removed by vacuum distillation. The product was then pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0038] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 202℃, 212℃, 225℃, 233℃, 233℃, 232℃, and 232℃, respectively, and the screw speed is 60 r / min.

[0039] Example 5 A composite flame-retardant nylon 6 material comprises the following raw materials: 85g nylon 6, 15g activated polyphenylene sulfide chopped fibers, 10g environmentally friendly flame retardant, 2g zinc borate, 3g SEBS-g-MAH, 3g acrylonitrile-styrene copolymer, 1.5g talc, 2g pentaerythritol phosphate, 2g nano-silica, 1.5g dodecyl stearic acid, 1.5g fatty amine polyoxyethylene ether, 2g ethylene bis-stearamide, and 1.5g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 1.5:1.

[0040] The environmentally friendly flame retardant is prepared by the following steps: 10g of DOPO flame retardant is added to 50g of anhydrous toluene and stirred evenly. 2g of vinyltriethoxysilane and 0.02g of AIBN are added. Under nitrogen protection, the mixture is heated to 85℃ and stirred for 4h. The solvent is removed by vacuum distillation. The product and 1.5g of γ-glycidyl etheroxypropyltrimethoxysilane are added to 50g of 60% ethanol aqueous solution. Triethylamine is added to adjust the pH of the system to 8-8.5. The mixture is stirred at 65℃ for 3h. The solvent is removed by vacuum distillation. The product is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0041] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 202℃, 212℃, 225℃, 233℃, 233℃, 232℃, and 232℃, respectively, and the screw speed is 60 r / min.

[0042] Comparative Example 1 A composite flame-retardant nylon 6 material comprises the following raw materials: 85g nylon 6, 15g activated polyphenylene sulfide chopped fibers, 10g environmentally friendly flame retardant, 2g zinc borate, 3g SEBS-g-MAH, 3g acrylonitrile-styrene copolymer, 1.5g talc, 2g pentaerythritol phosphate, 2g nano-silica, 1.5g dodecyl stearic acid, 1.5g fatty amine polyoxyethylene ether, 2g ethylene bis-stearamide, and 1.5g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 1.5:1.

[0043] The environmentally friendly flame retardant is prepared by the following steps: 10g of DOPO flame retardant and 1.5g of γ-glycidyl etheroxypropyltrimethoxysilane are added to 50g of 60% ethanol aqueous solution. Triethylamine is added to adjust the pH of the system to 8-8.5. The mixture is stirred at 65℃ for 3h, the solvent is removed by vacuum distillation, the mixture is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

[0044] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 202℃, 212℃, 225℃, 233℃, 233℃, 232℃, and 232℃, respectively, and the screw speed is 60 r / min.

[0045] Comparative Example 2 A composite flame-retardant nylon 6 material comprises the following raw materials: 85g nylon 6, 15g activated polyphenylene sulfide chopped fibers, 10g DOPO flame retardant, 2g zinc borate, 3g SEBS-g-MAH, 3g acrylonitrile-styrene copolymer, 1.5g talc, 2g pentaerythritol phosphate, 2g nano-silica, 1.5g dodecyl stearic acid, 1.5g fatty amine polyoxyethylene ether, 2g ethylene bis-stearamide, and 1.5g antioxidant. The antioxidant is composed of antioxidant 1010 and antioxidant 168 in a mass ratio of 1.5:1.

[0046] The preparation method of the above-mentioned composite flame-retardant nylon 6 material includes the following steps: mixing the raw materials evenly, and extruding and granulating them using a twin-screw extruder. The temperatures of each zone in the twin-screw extruder are 202℃, 212℃, 225℃, 233℃, 233℃, 232℃, and 232℃, respectively, and the screw speed is 60 r / min.

[0047] The tensile strength of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2 was determined in accordance with GB / T 1040.2-2022 "Determination of tensile properties of plastics - Part 2: Test conditions for molded and extruded plastics".

[0048] The flexural strength of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2 was determined in accordance with GB / T 9341-2008 "Determination of Flexural Properties of Plastics".

[0049] like Figure 1 As shown, the composite flame-retardant nylon 6 material obtained in Example 5 has the highest tensile strength and flexural strength, which are significantly better than those of Comparative Examples 1-2.

[0050] The notched impact strength of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2 was determined in accordance with GB / T 1043.1-2008 "Determination of impact properties of simply supported plastic beams - Part 1: Non-instrumental impact test".

[0051] The oxygen index of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2 was determined in accordance with GB / T 2406.2-2009 "Determination of flammability of plastics by oxygen index method - Part 2: Room temperature test".

[0052] like Figure 2 As shown, the composite flame-retardant nylon 6 material obtained in Example 5 has the highest notched impact strength and oxygen index, which are significantly better than those of Comparative Examples 1-2.

[0053] The UL94 flame retardancy ratings of the composite flame-retardant nylon 6 materials obtained in Example 5 and Comparative Examples 1-2 were determined. The flame retardancy rating of the composite flame-retardant nylon 6 material obtained in Example 5 was V-0, the flame retardancy rating of the composite flame-retardant nylon 6 material obtained in Comparative Example 1 was V-0, and the flame retardancy rating of the composite flame-retardant nylon 6 material obtained in Comparative Example 2 was V-2.

[0054] The present invention has been described in detail above. Those skilled in the art will recognize that the invention can be practiced in a wide range of ways with equivalent parameters, concentrations, and conditions without departing from its spirit and scope, and without requiring unnecessary experiments. While specific embodiments have been provided, it should be understood that further modifications can be made to the invention. In summary, according to the principles of the invention, this application is intended to include any changes, uses, or improvements to the invention, including changes made using conventional techniques known in the art that depart from the scope disclosed herein.

Claims

1. A composite flame-retardant nylon 6 material, characterized in that, The raw materials, by weight, include: 70-100 parts of nylon 6, 10-20 parts of activated polyphenylene sulfide chopped fiber, 5-15 parts of environmentally friendly flame retardant, 1-3 parts of flame retardant synergist, 1-5 parts of SEBS-g-MAH, 1-5 parts of acrylonitrile-styrene copolymer, 1-2 parts of talc, 1-3 parts of pentaerythritol phosphate, 1-3 parts of nano silica, 1-2 parts of dodecyl hydroxystearic acid, 1-2 parts of fatty amine polyoxyethylene ether, 1-3 parts of lubricant, and 1-2 parts of antioxidant. The raw materials for environmentally friendly flame retardants include: DOPO flame retardant, vinyltriethoxysilane, and γ-glycidoxypropyltrimethoxysilane.

2. The composite flame-retardant nylon 6 material according to claim 1, characterized in that, The flame retardant synergist is zinc borate.

3. The composite flame-retardant nylon 6 material according to claim 1, characterized in that, The lubricant is ethylene bis-stearamide.

4. The composite flame-retardant nylon 6 material according to claim 1, characterized in that, Antioxidants include: Antioxidant 1010, Antioxidant 168.

5. The composite flame-retardant nylon 6 material according to claim 4, characterized in that, The mass ratio of antioxidant 1010 to antioxidant 168 is 1-2:

1.

6. The composite flame-retardant nylon 6 material according to claim 1, characterized in that, The mass ratio of DOPO flame retardant, vinyltriethoxysilane, and γ-glycidyl etheroxypropyltrimethoxysilane is 5-10:1-4:1-2.

7. The composite flame-retardant nylon 6 material according to claim 1, characterized in that, The environmentally friendly flame retardant is prepared by the following steps: DOPO flame retardant is added to anhydrous toluene and stirred until homogeneous. Vinyltriethoxysilane and AIBN are added, and the mixture is heated to 80-90℃ and stirred for 2-6 hours under nitrogen protection. The solvent is removed, and the product is added to an ethanol aqueous solution along with γ-glycidoxypropyltrimethoxysilane. Triethylamine is added to adjust the pH of the system to 8-8.5, and the mixture is stirred at 50-70℃ for 2-4 hours. The solvent is removed, and the mixture is pulverized, washed, and vacuum dried to obtain the environmentally friendly flame retardant.

8. The composite flame-retardant nylon 6 material according to claim 7, characterized in that, The mass fraction of the ethanol aqueous solution is 40-60%.

9. A method for preparing a composite flame-retardant nylon 6 material as described in any one of claims 1-8, characterized in that, The process includes the following steps: mixing the raw materials evenly and extruding them into granules.

10. The method for preparing the composite flame-retardant nylon 6 material according to claim 9, characterized in that, Extrusion granulation was performed using a twin-screw extruder. The temperatures in each zone of the twin-screw extruder were 200-205℃, 210-215℃, 220-230℃, 230-235℃, 230-235℃, and 230-235℃, respectively, and the screw speed was 60-100 r / min.

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