Bromine-antimony flame-retardant reinforced and toughened plastic particles of nylon 66 and nylon 6 and preparation method of bromine-antimony flame-retardant reinforced and toughened plastic particles

The formulation and processing of nylon 66 and nylon 6 plastic particles with a bromine antimony composite addresses the issue of low strength and flame retardancy, resulting in improved plastic particles with enhanced properties.

CN120309996APending Publication Date: 2025-07-15ZHEJIANG DING SUPER POLYMER MATERIALS CO LTD
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Patent Information

Application Number
CN202510663892.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-22
Publication Date
2025-07-15

AI Technical Summary

Technical Problem

Existing plastic particles have shortcomings in strength, toughness and flame retardancy, and it is difficult to meet the requirements of high-quality products.

Method used

The method of producing bromine antimony-based flame retardant reinforced toughening plastic particles of nylon 66 and nylon 6 is adopted. By adding bromine antimony-based composite masterbatch, antioxidant, nucleating agent, toughening agent, flowing agent, mold release agent and dispersant, processing is carried out in a twin-screw high-twist extruder, controlling the temperature and vacuum evacuation, and finally detecting the ash in a muffle furnace, plastic particles with good dispersion are produced.

Benefits of technology

It improves the flame retardancy and strength of plastic particles, enhances its toughness, has good impact performance and aging resistance, color stability and fluidity.

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Abstract

The invention discloses bromine-antimony flame-retardant reinforced and toughened plastic particles of nylon 66 and nylon 6 and a manufacturing method of the bromine-antimony flame-retardant reinforced and toughened plastic particles, and the bromine-antimony flame-retardant reinforced and toughened plastic particles are characterized by comprising the following components in percentage by mass: 45-50% of nylon 6, 10-20% of nylon 66, 5-10% of SI02, 13-25% of bromine-antimony composite master batch, 0.1-0.2% of an antioxidant, 0.1-0.2% of a nucleating agent, 3-5% of a toughening agent, 0.2-0.5% of a flowable agent, 0.2-0.4% of a release agent and 0.1-0.3% of a dispersing agent. The flame-retardant plastic has the effects of good flame retardance, high strength and high toughness.
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Description

Technical Field

[0001] The present invention relates to the field of plastic particles, and more specifically, it relates to a bromine-antimony-based flame-retardant reinforced and toughened plastic particle of nylon 66 and nylon 6 and a manufacturing method thereof. Background Art

[0002] Plastic particles refer to granular plastics. Common plastic particles include general plastics, engineering plastics, and special plastics. General plastics include polypropylene, polyethylene, polyvinyl chloride, polystyrene, polyester, polyurethane, etc. Engineering plastics include nylon, polytetrafluoroethylene, polyoxymethylene, polycarbonate, silicone, etc. Special plastics include thermosetting plastics and functional polymer plastics. At present, some plastic particles are made of a single material, resulting in problems such as low strength, toughness, and flame retardancy in practical applications. As people's requirements for product quality are getting higher and higher, plastic particles used in various fields need to have high strength, toughness, and flame retardancy, thus requiring plastic particles to have high performance. Summary of the Invention

[0003] Aiming at the deficiencies of the existing technology, the present invention provides a bromine-antimony-based flame-retardant reinforced and toughened plastic particle of nylon 66 and 6 and a manufacturing method thereof, which have the effects of good flame retardancy, high strength, and high toughness.

[0004] To achieve the above object, the present invention provides the following technical solutions: A bromine-antimony-based flame-retardant reinforced and toughened plastic particle of nylon 66 and 6 and a manufacturing method thereof, including the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, bromine-antimony composite masterbatch, antioxidant, nucleating agent, toughening agent, flow agent, demolding agent, and dispersant into a blender, with a stirring speed of 900 revolutions per minute and a time of 1 - 3 minutes; Step 2: Pour the mixed material into a twin-screw high-torque extruder for strand cutting. The temperature range is set as follows: Zone 1: 220°C - 230°C; Zone 2: 240°C - 250°C; Zone 3: 240°C - 250°C; Zone 4: 220°C - 230°C; Zone 5: 220°C - 230°C; Zone 6: 220°C - 230°C, die head: 230°C - 240°C; main machine speed: 600 - 700 revolutions per minute, feeding speed: 2.3 - 2.4 revolutions per minute, current: 220A; Step 3: Add long glass fibers from the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The pumping force of the vacuum pump is 0.1 Mpa; Step 4: Regularly use a muffle furnace to detect the ash content of the particles during the strand cutting process, and control the error of the glass fiber content within 0.5%; Step 4: Pump the prepared plastic particles into a homogenizing tank, with a homogenizing time of 20 - 30 minutes and a homogenizing temperature of 70 - 85°C.

[0005] The present invention is further configured as follows: The muffle furnace detection method in step three is as follows: Use a scale with an accuracy of 0.01 to weigh 20 g of the product on a small iron plate, place it in the muffle furnace, set the temperature to 800 °C, burn for 10 minutes after reaching the set temperature, take it out with pliers and cool it, then measure the mass and divide it by 20 g to calculate the ash content.

[0006] The present invention is further configured as follows: The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is sodium 2,2 - methylenebis(4,6 - di - tert - butylphenyl) phosphate; the toughening agent is a POE toughening agent; the flow agent is calcium stearate; the release agent is a functional long - chain amide and methylsilane; the dispersant is fatty acid polyethylene glycol ester.

[0007] The present invention is further configured as follows: The production method of the bromine - antimony composite masterbatch is to add 10% by mass of polyethylene, 22.5% of antimony trioxide, and 67.5% of decabromodiphenylethane to a granulator and obtain it through the granulator.

[0008] The present invention is further configured as follows: A bromine - antimony - based flame - retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6 includes the following components by mass percentage: nylon 6: 45 - 50%, nylon 66: 10 - 20%, SiO₂: 5 - 10%, bromine - antimony composite masterbatch: 13 - 25%, antioxidant: 0.1 - 0.2%, nucleating agent: 0.1 - 0.2%, toughening agent: 3 - 5%, flow agent: 0.2 - 0.5%, release agent: 0.2 - 0.4%, dispersant: 0.1 - 0.3%.

[0009] In summary, the present invention has the following beneficial effects: The bromine - antimony composite masterbatch is used in the plastic particles, which has good dispersibility, more stable product color change, stronger impact performance and flame - retardant performance, thus making the plastic particles have good flame retardancy. The POE toughening agent enhances the toughness and strength of the plastic particles through characteristics such as physical cross - linking points, aging resistance, compatibility, and fluidity; sodium 2,2 - methylenebis(4,6 - di - tert - butylphenyl) phosphate can accelerate the crystallization rate; the characteristics of high strength, rigidity, wear resistance, heat resistance, chemical stability, and self - lubricity of nylon 6 and nylon 66 further improve the strength and toughness of the plastic particles. Specific Embodiments

[0010] The following further elaborates on the present invention with reference to embodiments. Embodiment

[0011] A production method of a bromine - antimony - based flame - retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6 includes the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, bromine-antimony composite masterbatch, antioxidant, nucleating agent, toughening agent, flow agent, demolding agent, and dispersant into a blender, and stir at a speed of 900 revolutions per minute for 1 minute. Step 2: Pour the mixed materials into a twin-screw high-torque extruder for strand cutting. The temperature range is set as follows: Zone 1: 222 °C; Zone 2: 244 °C; Zone 3: 242 °C; Zone 4: 225 °C; Zone 5: 224 °C; Zone 6: 220 °C, die head: 230 °C; main machine speed: 650 revolutions per minute, feeding speed: 2.3 revolutions per minute, current: 220 A. Step 3: Add long glass fiber from the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The pumping force of the vacuum pump is 0.1 Mpa. Step 4: During the strand cutting process, regularly use a muffle furnace to detect the ash content of the particles, and control the error of the glass fiber content within 0.5%. Step 4: Pump the prepared plastic particles into a homogenizing tank. The homogenizing time is 20 minutes, and the homogenizing temperature is 75 °C.

[0012] The muffle furnace detection method in Step 3 is as follows: Use a scale with a precision of 0.01 to weigh 20 g of the product on a small iron tray, put it into the muffle furnace, set the temperature to 800 °C, burn for 10 minutes after reaching the set temperature, take it out with pliers to cool, and then divide the measured mass by 20 g to calculate the ash content.

[0013] The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is 2,2 - methylenebis(4,6 - di - tert - butylphenyl) sodium phosphate; the toughening agent is POE toughening agent; the flow agent is calcium stearate; the demolding agent is a functional long-chain amide; the dispersant is fatty acid polyethylene glycol ester.

[0014] The production method of the bromine-antimony composite masterbatch is to add 10% by mass of polyethylene, 22.5% of antimony trioxide, and 67.5% of decabromodiphenylethane into a granulator and obtain it through the granulator.

[0015] A bromine-antimony series flame-retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6 includes the following components by mass percentage: nylon 6: 46.4%, nylon 66: 18%, SiO₂: 8%, bromine-antimony composite masterbatch: 21%, antioxidant: 0.2%, nucleating agent: 0.2%, toughening agent: 5%, flow agent: 0.5%, demolding agent: 0.4%, dispersant: 0.3%. Example

[0016] A production method of a bromine-antimony series flame-retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6 includes the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, bromine-antimony composite masterbatch, antioxidant, nucleating agent, toughening agent, flow agent, demolding agent, and dispersant into a blender, with a stirring speed of 900 revolutions per minute for 2 minutes; Step 2: Pour the mixed materials into a twin-screw high-torque extruder for strand cutting. The temperature range is set as follows: Zone 1: 224°C; Zone 2: 248°C; Zone 3: 247°C; Zone 4: 226°C; Zone 5: 224°C; Zone 6: 225°C, die head: 232°C; main machine speed: 660 revolutions per minute, feeding speed: 2.4 revolutions per minute, current: 220A; Step 3: Add long glass fibers through the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The pumping force of the vacuum pump is 0.1 Mpa; Step 4: During the strand cutting process, regularly use a muffle furnace to detect the ash content of the particles, and control the error of the glass fiber content within 0.5%;

[0017] Step 4: Pump the prepared plastic particles into a homogenizing tank, with a homogenizing time of 25 minutes and a homogenizing temperature of 80°C.

[0018] The muffle furnace detection method in Step 3 is as follows: Use a scale with a precision of 0.01 to weigh 20 g of the product on a small iron tray, put it into the muffle furnace, set the temperature to 800°C, burn for 10 minutes after reaching the set temperature, take it out with pliers to cool, and then divide the measured mass by 20 g to calculate the ash content.

[0019] The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is 2,2 - methylenebis(4,6 - di - tert - butylphenyl) sodium phosphate; the toughening agent is POE toughening agent; the flow agent is calcium stearate; the demolding agent is methyl silane; the dispersant is fatty acid polyethylene glycol ester.

[0020] A bromine - antimony - based flame - retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6, by mass percentage, includes the following components: nylon 6: 46.8%, nylon 66: 15%, SiO₂: 10%, bromine - antimony composite masterbatch: 22%, antioxidant: 0.2%, nucleating agent: 0.1%, toughening agent: 5%, flow agent: 0.3%, demolding agent: 0.4%, dispersant: 0.2%. Example

[0021] A manufacturing method of a bromine - antimony - based flame - retardant, reinforced, and toughened plastic particle of nylon 66 and nylon 6, includes the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, bromine - antimony composite masterbatch, antioxidant, nucleating agent, toughening agent, flow agent, demolding agent, and dispersant into a blender, with a stirring speed of 900 revolutions per minute for 3 minutes; Step 2: Pour the mixed materials into a twin-screw high-torque extruder for strand pelletizing. The temperature range is set as follows: Zone 1: 227°C; Zone 2: 240°C; Zone 3: 244°C; Zone 4: 227°C; Zone 5: 225°C; Zone 6: 228°C, die head: 233°C; main machine speed: 670 rpm, feeding speed: 2.4 rpm, current: 220 A; Step 3: Add long glass fibers from the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The suction force of the vacuum pump is 0.1 Mpa; Step 4: During the strand pelletizing process, regularly use a muffle furnace to detect the ash content of the pellets, and control the error of the glass fiber content within 0.5%; Step 4: Pump the produced plastic pellets into a homogenizing tank. The homogenizing time is 24 minutes and the homogenizing temperature is 80°C.

[0022] The muffle furnace detection method in Step 3 is as follows: Use a scale with a precision of 0.01 to weigh 20 g of the product on a small iron tray, put it into the muffle furnace, set the temperature to 800°C, burn for 10 minutes after reaching the set temperature, take it out with pliers and cool it, then divide the measured mass by 20 g to calculate the ash content.

[0023] The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is 2,2'-methylenebis(4,6-di-tert-butylphenyl) sodium phosphate; the toughening agent is POE toughening agent; the flow agent is calcium stearate; the release agent is methylsilane; the dispersant is fatty acid polyethylene glycol ester.

[0024] The production method of the bromine-antimony composite masterbatch is to add 10% by mass of polyethylene, 22.5% of antimony trioxide, and 67.5% of decabromodiphenylethane to a granulator and obtain it through the granulator.

[0025] A bromine-antimony-based flame-retardant reinforced and toughened plastic pellet of nylon 66 and nylon 6 includes the following components by mass percentage: nylon 6: 48.9%, nylon 66: 18%, SiO2: 9%, bromine-antimony composite masterbatch: 19%, antioxidant: 0.1%, nucleating agent: 0.1%, toughening agent: 4%, flow agent: 0.4%, release agent: 0.2%, dispersant: 0.3%. Example

[0026] A production method of a bromine-antimony-based flame-retardant reinforced and toughened plastic pellet of nylon 66 and nylon 6 includes the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, and decabromodiphenyl ether, antimony trioxide, antioxidant, nucleating agent, toughening agent, flow agent, release agent, and dispersant to a mixer. The stirring speed is 900 rpm and the time is 3 minutes; Step 2: Pour the mixed materials into a twin-screw high-torque extruder for strand pelletizing. The temperature range is set as follows: Zone 1: 228°C; Zone 2: 246°C; Zone 3: 243°C; Zone 4: 225°C; Zone 5: 226°C; Zone 6: 230°C, die head: 240°C; main machine speed: 640 rpm, feeding speed: 2.4 rpm, current: 220 A; Step 3: Add long glass fibers from the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The pumping force of the vacuum pump is 0.1 Mpa; Step 4: During the strand pelletizing process, regularly use a muffle furnace to detect the ash content of the pellets, and control the error of the glass fiber content within 0.5%; Step 4: Pump the produced plastic pellets into the homogenization tank. The homogenization time is 25 minutes and the homogenization temperature is 83°C.

[0027] The detection method of the muffle furnace in Step 3 is as follows: Use a scale with a precision of 0.01 to weigh 20 g of the product on a small iron tray, put it into the muffle furnace, set the temperature to 800°C, burn for 10 minutes after reaching the set temperature, take it out with pliers and cool it, then measure the mass and divide by 20 g to calculate the ash content.

[0028] The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is sodium 2,2'-methylenebis(4,6-di-tert-butylphenyl) phosphate; the toughening agent is POE toughening agent; the flow agent is calcium stearate; the demolding agent is methyl silane; the dispersant is fatty acid polyethylene glycol ester.

[0029] The production method of the bromine-antimony composite masterbatch is to add 10% by mass of polyethylene, 22.5% of antimony trioxide, and 67.5% of decabromodiphenylethane to a granulator and obtain it through the granulator.

[0030] A bromine-antimony series flame-retardant reinforced and toughened plastic pellet of nylon 66 and nylon 6 includes the following components by mass percentage: nylon 6: 47%, nylon 66: 11.6%, SiO₂: 10%, bromine-antimony composite masterbatch: 25%, antioxidant: 0.2%, nucleating agent: 0.2%, toughening agent: 5%, flow agent: 0.5%, demolding agent: 0.4%, dispersant: 0.1%.

[0031] Comparative Example 1: This example provides a bromine-antimony series flame-retardant reinforced and toughened plastic pellet of nylon 66 and nylon 6 and its production method.

[0032] This comparative example is compared with Example 1, in which only antimony trioxide is added as a flame retardant, and the rest of the steps are the same as those in Example 1.

[0033] Comparative Example 2: This embodiment provides a bromine-antimony-based flame-retardant, reinforced and toughened plastic particle of nylon 66 and nylon 6 and a manufacturing method thereof.

[0034] This comparative example is compared with Example 1, in which only decabromodiphenylethane is added as the flame retardant, and the remaining steps are the same as those in Example 1.

[0035] The following is the performance table of each embodiment: Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Flame retardancy V0 V0 V0 V0 V1 V1 Tensile strength MPa 107 105 104 110 99 100 Impact strength KJ / m² 9.5 9.4 9.5 9.3 8.8 8.7 According to the table, it can be seen that the plastic particles prepared in Examples 1-4 have good flame retardancy and mechanical properties, and each property is higher than those in Comparative Examples 1-2. From Example 1 and Comparative Example 1, it can be seen that the bromine-antimony composite masterbatch added in Example 1 has good flame retardancy and dispersion properties, thus being able to improve the flame retardancy and mechanical properties of the plastic particles; from Example 1, Comparative Example 1 and Comparative Example 2, it can be known that the bromine-antimony composite masterbatch prepared in the present invention has better flame retardant effect compared with antimony trioxide and decabromodiphenylethane, and it can also prove that the bromine-antimony composite masterbatch can make each component uniformly disperse on the plastic particles, that is, it has good dispersion, thereby improving the various properties of the plastic particles.

[0036] The above are only the preferred embodiments of the present invention, and are not used to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the design concept of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for preparing nylon 66 and nylon 6 bromine-antimony based flame retardant reinforced and toughened plastic particles, characterized in that: It includes the following steps: Step 1: Add nylon 6 chips, nylon 66 chips, bromine-antimony composite masterbatch, antioxidant, nucleating agent, toughening agent, flow agent, demolding agent, and dispersant into a blender, with a stirring speed of 900 revolutions per minute for 1 - 3 minutes; Step 2: Pour the mixed material into a twin-screw high-torque extruder for strand cutting. The temperature range is set as follows: Zone 1: 220°C - 230°C; Zone 2: 240°C - 250°C; Zone 3: 240°C - 250°C; Zone 4: 220°C - 230°C; Zone 5: 220°C - 230°C; Zone 6: 220°C - 230°C, die head: 230°C - 240°C; main machine speed: 600 - 700 revolutions per minute, feeding speed: 2.3 - 2.4 revolutions per minute, current: 220A; Step 3: Add long glass fibers from the glass fiber port on the twin-screw high-torque extruder and turn on the vacuum pump to evacuate. The pumping force of the vacuum pump is 0.1 Mpa; Step 4: Regularly use a muffle furnace to detect the ash content of the particles during the strand cutting process, and control the error of the glass fiber content within 0.5%; Step 4: Pump the prepared plastic particles into a homogenizing tank. The homogenizing time is 20 - 30 minutes, and the homogenizing temperature is 70 - 85°C.

2. The manufacturing method of the nylon 66 and nylon 6 bromine-antimony flame retardant reinforced and toughened plastic particles according to claim 1, characterized in that: The muffle furnace detection method in Step 3 is as follows: Use a scale with a precision of 0.01 to weigh 20 g of the product on a small iron plate, put it into the muffle furnace, set the temperature to 800°C, burn for 10 minutes after reaching the set temperature, take it out with pliers to cool, and then divide the measured mass by 20 g to calculate the ash content.

3. The manufacturing method of the bromine-antimony-based flame-retardant reinforced and toughened plastic particles of nylon 66 and nylon 6 according to claim 1, wherein: The antioxidant is antioxidant 168 and antioxidant 1010; the nucleating agent is sodium 2,2'-methylenebis(4,6-di-tert-butylphenyl) phosphate, which is an efficient nucleating agent that can change the crystallinity of incompletely crystalline polymers and accelerate their crystallization rate.; The toughening agent is POE toughening agent; the flow agent is calcium stearate; the demolding agent is long-chain amide functional group and methylsilane; the dispersant is fatty acid polyethylene glycol ester.

4. The manufacturing method of the bromine-antimony-based flame-retardant reinforced and toughened plastic particles of nylon 66 and nylon 6 according to claim 1, characterized in that: The production method of the bromine-antimony composite masterbatch is to add 10% by mass percentage of polyethylene, 22.5% of antimony trioxide, and 67.5% of decabromodiphenylethane into a granulator and obtain it through the granulator.

5. A bromine-antimony based flame retardant reinforced and toughened plastic particle of nylon 66 and nylon 6, characterized in that: It includes the following components by mass percentage: nylon 6: 45 - 50%, nylon 66: 10 - 20%, SiO₂: 5 - 10%, bromine-antimony composite masterbatch: 13 - 25%, antioxidant: 0.1 - 0.2%, nucleating agent: 0.1 - 0.2%, toughening agent: 3 - 5%, flow agent: 0.2 - 0.5%, demolding agent: 0.2 - 0.4%, dispersant: 0.1 - 0.3%.