Low-odor glass fiber reinforced nylon modified material and preparation method thereof
By adding carbon adsorbent and aminosilane coupling agent to modify glass fiber in nylon material, and combining multiple polymerization and high-temperature extraction treatment, the problem of strong odor in nylon material during processing was solved, achieving low odor and excellent physical properties.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGSU PUFEIER PLASTIC TECH CO LTD
- Filing Date
- 2020-04-28
- Publication Date
- 2026-04-17
AI Technical Summary
Existing nylon materials are prone to releasing monomers and oligomers during processing, resulting in a strong odor and affecting their application in automotive interior parts.
By adding carbon powder as an adsorbent to nylon material and performing vacuum treatment during multiple polymerization and extrusion processes, combined with aminosilane coupling agent to modify glass fiber, residual monomers and oligomers are reduced. The huge specific surface area of carbon powder is used for physical adsorption, and odor is removed by high-temperature extraction.
It significantly reduces the odor of nylon materials, meets the low-odor requirement, and improves the physical and processing properties of the materials.
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Figure CN111349336B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to nylon materials, specifically to a glass fiber modified nylon material for reinforcement purposes, and more specifically to nylon 6 (PA6) granules. Background Technology
[0002] Nylon (PA), also known as polyamide, with Nylon 6 (PA6) being a polymer boasting excellent comprehensive properties, including superior mechanical properties, excellent solvent resistance, and oil resistance, making it widely used in the automotive industry. However, PA6 leaves residual monomers and oligomers during polymerization, leading to the easy precipitation of these monomers and oligomers during processing. This results in a strong odor problem for PA6-based modified materials used in automotive interior parts.
[0003] Publication No. CN101314672A discloses a high-gloss, low-odor, reinforced nylon composite material and its preparation method. The composite material is composed of the following components by weight percentage: PA66 resin, PA6 resin, glass fiber, inorganic minerals, microspheres, compatibilizer, antioxidant, lubricant, etc. The various raw materials are mixed in a high-speed mixer; discharged; and granulated. The PA composite material prepared by this method has advantages such as high gloss, good strength, and low odor. 1. Adding microspheres and barium sulfate to the glass fiber and mineral-reinforced nylon materials makes the product surface smooth and glossy, and improves processing performance. 2. Adding zinc sulfide, maleic anhydride grafts, and lubricants to the glass fiber and mineral-reinforced nylon materials reduces the odor emitted during processing. 3. Using both glass fiber and inorganic minerals as fillers, the two fillers complement each other, resulting in excellent comprehensive performance of the material.
[0004] Publication No. CN102558839A discloses a low-odor, antistatic, red phosphorus flame-retardant thermoplastic composition and its preparation method. The raw materials are formulated as follows: 40-60% nylon resin; 5-10% microencapsulated red phosphorus masterbatch; 3-8% compatibilizer; 5-40% filler; 1-5% modified activated zeolite powder; 0.5-2% nano-magnesium hydroxide; and 0-5% other additives. The modified activated zeolite powder is natural zeolite powder activated and then modified with a cationic surfactant. This invention, by adding modified activated zeolite powder to the basic formulation of a red phosphorus flame-retardant thermoplastic composition, prepares a low-odor, antistatic, and highly stable red phosphorus flame-retardant thermoplastic composition, which also has a certain antibacterial effect. This thermoplastic composition can be extruded to form various samples, suitable for coal mine equipment, textile equipment, and medical devices.
[0005] Publication No. CN109666216A discloses a high-strength, low-odor long glass fiber reinforced polypropylene / polyamide alloy material and its preparation method. This alloy material is specifically prepared from the following components in the following weight ratios: 20-65 parts nylon 6 or nylon 66, 5-25 parts polyamide, 20-60 parts continuous glass fiber, 1-3 parts maleic anhydride compatibilizer, 1-15 parts long-chain polyamide, 0.5-1.5 parts color masterbatch, 0.2-0.6 parts antioxidant, and 0.1-0.5 parts crosslinking agent. According to popular odor standards, the long glass fiber reinforced polypropylene / polyamide alloy material of this invention reduces odor by 0.5-1 level. In the alloy composite material of this invention, by limiting the specific ratio of polypropylene and polyamide, a resin alloy system with good compatibility can be obtained. Furthermore, the addition of long-chain polyamide in the formulation of this invention effectively reduces the amount of compatibilizer used, thereby improving the product odor.
[0006] Publication No. CN110655781A discloses a low-odor, high-wear-resistant nylon material and its preparation method, comprising the following components: nylon 6, nylon 1010, POE-grafted maleic anhydride, poly(p-benzoamide) modified glass fiber, odor-absorbing masterbatch, a mixture of silicon nitride and silicon carbide, lubricant, and antioxidant. The addition of odor-absorbing masterbatch in this invention significantly improves the odor and emission characteristics of the material, resulting in a TVOC of less than 40 μgC / g for the nylon 6 composition. The odor-absorbing masterbatch comprises: 100 parts nylon 66, 5 parts hydrophobic diatomaceous earth, 5 parts hydrophobic activated carbon, 5 parts needle-like zeolite molecular sieve, 5 parts zinc ricinoleate, 5 parts nano-silica, 1 part calcium stearate, and 5 parts melamine. The odor-absorbing masterbatch in this literature uses nylon as the matrix, improving its compatibility with fibers and nylon 66, and ensuring the dispersibility of the masterbatch in the composition system.
[0007] Currently, those skilled in the art mainly suppress odor sources through the compatibility of raw materials. Some require the addition of inorganic fillers such as minerals, microspheres, zeolite molecular sieves, and carbon powder to nylon base materials, or the addition of organic auxiliaries that help with polymerization or expansion of molecular chains. The addition of these additives or auxiliaries will more or less affect the physical properties of nylon materials, and even affect the original application of the materials. Summary of the Invention
[0008] The purpose of this invention is to provide a method for preparing low-odor glass fiber reinforced nylon materials, and more specifically, a method for producing low-odor glass fiber reinforced modified PA6: on the one hand, carbon powder is added to the composition as an adsorbent, and its huge specific surface area is used to physically adsorb odor; on the other hand, the preparation method is designed to reduce residual monomers and oligomers.
[0009] The technical solution adopted by this invention to solve the above problems is as follows: a low-odor glass fiber reinforced nylon modified material, mainly prepared from the following raw materials in weight fractions:
[0010] PA6 sections 60-80%
[0011] 20-40% glass fiber
[0012] Additives 0.1-0.2%,
[0013] Carbon powder 1.0-2.0%,
[0014] The carbon powder serves as both a black masterbatch and an odor adsorbent. Preferably, it is the carbon powder used in inks, exhibiting finer particle size and a larger specific surface area. The relative viscosity of the PA6 chips in the raw material is 2.37-2.47, and the moisture content is 0.25-0.5%. The length of the glass fiber in the raw material is 3.0±1.0 mm.
[0015] The additives are selected from one or more of antioxidants, lubricants, and catalysts.
[0016] The core of this invention lies in a method for preparing a low-odor glass fiber reinforced nylon modified material, comprising the following steps:
[0017] (1) Immerse glass fibers in an aminosilane coupling agent dispersion;
[0018] (2) Mix PA6 chips, additives and carbon powder and add them to the high pressure polymerizer from the main material port. Filter the dispersion system of step (1), take the filter residue (glass fiber modified with aminosilane coupling agent) and add it to the high pressure polymerizer. At the same time, add deionized water accounting for 0.8-2% of PA6 content, seal the reactor, pressurize and react for 3-7 hours. The reaction pressure is 6-12MPa and the reaction temperature is 200-280℃. After the reaction is completed, discharge the material and dry it at 60-80℃ for more than 2 hours.
[0019] (3) Transfer the reactants from step (2) to another polymerization reactor, evacuate and depressurize, bringing the pressure down to 1×10⁻⁶. 3 After the Pa is below, start heating and set the reaction temperature to 160-220℃. Turn on the cooling to maintain the reaction temperature and react for 8-12 hours. Then, discharge the melt through the screw, extrude it through the wire casting head, cool it in the cooling bath and cut it into pellets. After pelleting, it enters the 80℃-100℃ high-temperature extraction elevator.
[0020] (4) Dry the granules from step (3) in a vacuum oven, feed the material into a twin-screw extruder, turn on the vacuum pump of the extruder, set a film forming device at the top of the barrel, and set the temperature of the twin-screw extruder as follows: Zone 1: 250-270℃, Zone 2: 250-270℃, Zone 3: 240-260℃, Zone 4: 230-250℃, Zone 5: 220-240℃, Zone 6: 220-240℃, Zone 7: 220-240℃, Zone 8: 220-240℃, Zone 9: 230-250℃;
[0021] (5) After the material is discharged from the extruder, it enters the 20-30℃ cooling water tank, then enters the pelletizer with a speed of 700-1200r / min, and after being screened by the vibrating screen, it enters the 80℃-100℃ high temperature extraction elevator, and finally enters the homogenization chamber.
[0022] Preferably, the wetting and dispersing agent is aminoethylaminopropyltrimethoxysilane, KH550 silane coupling agent, KH560 silane coupling agent, or KH570 silane coupling agent. Among these aminosilane coupling agents, aminoethylaminopropyltrimethoxysilane is particularly effective.
[0023] This application modifies glass fiber grafting using an aminosilane coupling agent. After filtration, drying is unnecessary; the modified glass fiber is then mixed with PA6 and becomes hydrophilic. During the first polymerization reaction, some of the residual oligomers and PA monomers in the PA6 chips undergo addition with the polymer, causing chain extension. The oligomers and PA monomers that do not participate in the addition reaction undergo ring-opening reactions under hydrolysis, with the monomers opening into aminohexanoic acid. Generally, the residual oligomers are mainly cyclic dimers, which open into carboxyl-terminated dimers. By modifying the glass fiber with hydrophilicity, the glass fiber incorporates water into the PA matrix through melt mixing, maximizing the promotion of ring-opening of oligomers and monomers in the PA matrix.
[0024] Clearly, the first polymerization reaction increased the water content of the PA matrix to 1.2-2.1%, a significant increase compared to PA chips. High water content is detrimental to the condensation polymerization reaction. Condensation polymerization of aminocaproic acid, carboxyl-terminated dimers, and oligomers all produce water as a byproduct, and the reaction is continuously exothermic. To promote the condensation polymerization reaction, the second polymerization reaction requires lowering the reaction temperature, applying a vacuum, and extending the reaction time. During the reaction, the viscosity increases, and the reaction system is continuously evacuated, causing water vapor to continuously precipitate out and carry away odors, thus achieving the first deodorization.
[0025] After the second polymerization reaction, the pellets are extruded through a cast strip and immediately subjected to high-temperature extraction to remove precipitates and achieve a second deodorization process. The third polymerization is achieved through a twin-screw extruder, combined with vacuuming and a film-forming device to further remove moisture from the polymerization system. After pelleting, the pellets undergo another high-temperature extraction process. Attached Figure Description
[0026] Figure 1 This is a schematic diagram of the structure of the drying, deodorizing, and deodorizing machine involved in the embodiments of the present invention;
[0027] Figure 2 This is a cross-sectional view of the deodorization and odor removal machine involved in the embodiments of the present invention;
[0028] In the attached diagram, 1-Volatile deodorization device, 2-Screw elevator, 101-Volatile deodorization cylinder, 102-Heating cylinder, 103-Waste heat recovery cylinder, 104-Support, 105-Outlet pipe, 106-Blower, 107-Inlet pipe, 108-Fixed platform, 109-Column, 110-Heater, 111-Outlet pipe, 112-Flow valve, 113-Support, 114-Motor, 115-Shaft, 116-First carbon adsorption cylinder, 117-Second carbon adsorption cylinder, 201-Inlet pipe, 202-First inclined pipe, 203-Second inclined pipe, 204-Platform, 205-Support leg. Detailed Implementation
[0029] The present invention will be further described in detail below with reference to the embodiments. The embodiments are exemplary and intended to explain the present invention, but should not be construed as limiting the present invention.
[0030] Example 1
[0031] The modified nylon material is prepared according to the following steps.
[0032] (1) Prepare the raw materials:
[0033] PA6 sections 70%
[0034] Modified glass fiber 28%,
[0035] Silicon carbide lubricant 0.2%,
[0036] Carbon powder 1.8%,
[0037] PA6 chips have an average molecular weight of 8,000-20,000 and a water content of 0.32%.
[0038] The glass fiber has a length of 3.0±1.0 mm. The glass fiber is immersed in an aqueous solution of aminoethylaminopropyltrimethoxysilane for 48 hours, filtered, and the filter residue is dried for later use.
[0039] (2) After mixing PA6 chips, additives, carbon powder and modified glass fiber, add them to the high-pressure polymerizer through the main material port. At the same time, add deionized water accounting for 1% of the PA6 content, seal the reactor, and pressurize for 6 hours. The reaction pressure is 7-8 MPa and the reaction temperature is 240-260℃. After the reaction is completed, discharge the material and dry it at 60-80℃ for more than 2 hours.
[0040] (3) Transfer the reactants from step (2) to another polymerization reactor, turn on the vacuum pump to reduce the pressure to 1×10⁻⁶. 3 After the Pa is below, the temperature is raised. The reaction temperature is set to 180-200℃. Once the temperature is reached, the water cooling device is turned on to maintain the reaction temperature. The reaction is carried out for 10 hours. The discharge port of the polymerization reactor is selected to discharge the melt through the screw. The melt is extruded through the wire casting head, cooled and pelletized in a cooling bath, and the pellets are extracted at a high temperature of 80℃-100℃ to remove the precipitates.
[0041] (4) Dry the granules from step (3) in a vacuum oven at a temperature of 100-120°C. Feed the material into a twin-screw extruder, turn on the vacuum pump of the extruder, and set a film-forming device at the top of the barrel. Set the temperature of the twin-screw extruder as follows: Zone 1: 250-270°C, Zone 2: 250-270°C, Zone 3: 240-260°C, Zone 4: 230-250°C, Zone 5: 220-240°C, Zone 6: 220-240°C, Zone 7: 220-240°C, Zone 8: 220-240°C, and Zone 9: 230-250°C.
[0042] (5) After the material is discharged from the extruder, it is cooled in a cooling water tank at 20-30℃ and then enters a pelletizer with a speed of 700-1200r / min. After being screened by a vibrating screen, it undergoes high-temperature steam extraction at 80℃-100℃.
[0043] (6) Drying and removing the devolatilization from the granules.
[0044] Example 2
[0045] The modified nylon material is prepared according to the following steps.
[0046] (1) Prepare the raw materials:
[0047] PA6 sections 65%
[0048] Modified glass fiber 32%,
[0049] Antioxidant 1010 0.2%,
[0050] Carbon powder 1.8%,
[0051] PA6 chips have an average molecular weight of 8,000-20,000 and a water content of 0.32%.
[0052] The glass fibers had a length of 3.0 ± 1.0 mm. The fibers were impregnated in an aqueous solution of aminoethylaminopropyltrimethoxysilane for 48 hours, then filtered and dried.
[0053] (2) Mix PA6 chips, additives and carbon powder and add them to the polymerization high pressure reactor from the main material port. Filter the dispersion system of step (1), take the filter residue and add it to the polymerization high pressure reactor. At the same time, add deionized water accounting for 0.8-2% of PA6 content. Seal the reactor and pressurize the reaction for 3-7 hours. The reaction pressure is 10-12MPa and the reaction temperature is 200-280℃. After the reaction is completed, discharge the material and dry it at 60-80℃ for more than 2 hours.
[0054] (3) Transfer the reactants from step (2) to another polymerization reactor, evacuate and depressurize, bringing the pressure down to 1×10⁻⁶. 3 After the Pa is below, start heating and set the reaction temperature to 160-220℃. Turn on the cooling to maintain the reaction temperature and react for 12 hours. The melt is discharged through the screw and extruded through the wire casting head. It is cooled and granulated in the cooling bath. The granules are then extracted and improved at a high temperature of 80℃-100℃.
[0055] (4) Dry the granules from step (3) in a vacuum oven at a temperature of 100-120°C. Feed the material into a twin-screw extruder, turn on the vacuum pump of the extruder, and set a film-forming device at the top of the barrel. Set the temperature of the twin-screw extruder as follows: Zone 1: 250-270°C, Zone 2: 250-270°C, Zone 3: 240-260°C, Zone 4: 230-250°C, Zone 5: 220-240°C, Zone 6: 220-240°C, Zone 7: 220-240°C, Zone 8: 220-240°C, and Zone 9: 230-250°C.
[0056] (5) After the material is discharged from the extruder, it is cooled in a cooling water tank at 20-30℃ and then enters a pelletizer with a speed of 700-1200r / min. After being screened by a vibrating screen, it undergoes high-temperature steam extraction at 80℃-100℃.
[0057] (6) Drying and removing the devolatilization from the granules.
[0058] Example 3
[0059] The modified nylon material is prepared according to the following steps.
[0060] (1) Prepare the raw materials:
[0061] PA6 sections 78%
[0062] Modified glass fiber 20%,
[0063] Antioxidant 1010 0.2%,
[0064] Zinc oxide 0.02%
[0065] Carbon powder 1.6%,
[0066] PA6 chips have an average molecular weight of 8,000-20,000 and a water content of 0.32%.
[0067] The glass fibers had a length of 3.0 ± 1.0 mm. The fibers were impregnated in an aqueous solution of aminoethylaminopropyltrimethoxysilane for 48 hours, then filtered and dried.
[0068] (2) Mix PA6 chips, additives and carbon powder and add them to the polymerization high pressure reactor from the main material port. Filter the dispersion system of step (1), take the filter residue and add it to the polymerization high pressure reactor. At the same time, add deionized water accounting for 1.2% of PA6 content. Seal the reactor and pressurize it for 7 hours. The reaction pressure is 6-9 MPa and the reaction temperature is 260-280℃. After the reaction is completed, discharge the material and dry it at 60-80℃ for more than 2 hours.
[0069] (3) Transfer the reactants from step (2) to another polymerization reactor, evacuate and depressurize, bringing the pressure down to 1×10⁻⁶. 3 After the Pa is below, start heating and set the reaction temperature to 160-180℃. Turn on the cooling to maintain the reaction temperature and react for 8 hours. The melt is discharged through the screw and extruded through the wire casting head. It is cooled and granulated in the cooling bath. The granules are then extracted and improved at a high temperature of 80℃-100℃.
[0070] (4) Dry the granules from step (3) in a vacuum oven, feed the material into a twin-screw extruder, turn on the vacuum pump of the extruder, set a film forming device at the top of the barrel, and set the temperature of the twin-screw extruder as follows: Zone 1: 250-270℃, Zone 2: 250-270℃, Zone 3: 240-260℃, Zone 4: 230-250℃, Zone 5: 220-240℃, Zone 6: 220-240℃, Zone 7: 220-240℃, Zone 8: 220-240℃, Zone 9: 230-250℃;
[0071] (5) After the material is discharged from the extruder, it enters a cooling water tank at 20-30℃ for cooling, and then enters a pelletizer at a speed of 700-1200r / min. After being screened by a vibrating screen, it undergoes high-temperature steam extraction at 80℃-100℃.
[0072] (6) Drying and removing the devolatilization from the granules.
[0073] The physical property test results of Examples 1-3 are as follows:
[0074]
[0075] The odor detection results of Examples 1-3 are as follows:
[0076] Humid (23℃, 24h) Humid state (40℃, 24h) Dry state (80℃, 24h) Example 1 2.0 2.5 3.0 Example 2 2.0 2.5 3.0 Example 3 2.0 3.0 3.5 Odor rating 2.0 2.5 3.0 Require ≤3.0 ≤3.0 ≤3.5
[0077] Odor Rating Chart
[0078] grade Evaluation criteria 1.0 Imperceptible odor 2.0 Detectable, with no unpleasant odor 3.0 Clearly identifiable, with no unpleasant odor. 4.0 Unpleasant odor 5.0 Severely unpleasant odor 6.0 Unbearable smell
[0079] The drying and devolatilization of the granules in this application are completed on a machine, the structure of which is described as follows:
[0080] A drying deodorization and deodorization machine for the production of modified nylon materials includes a deodorization and deodorization device 1 and a screw conveyor 2. The deodorization and deodorization device 1 includes a deodorization and deodorization cylinder 101, a heating cylinder 102 is fixedly connected to the bottom of the deodorization and deodorization cylinder 101, and a waste heat recovery cylinder 103 is fixedly connected to the bottom of the heating cylinder 102.
[0081] The bottom periphery of the screw conveyor 2 is fixedly connected to the feed pipe 201. The top periphery of the screw conveyor 2 and the top of the deodorization and odor removal cylinder 101 are fixedly connected to the first inclined pipe 202. The periphery of the waste heat recovery cylinder 103 and the bottom periphery of the screw conveyor 2 are fixedly connected to the second inclined pipe 203. The screw conveyor 2 includes a shell. A drive motor is fixedly installed on the top of the shell. One end of the output shaft of the drive motor passes through the top of the shell and is fixedly connected to a spiral auger. The bottom end of the spiral auger is rotatably connected to the bottom of the shell through a bearing. The drive motor drives the spiral auger to rotate, thereby realizing the upward conveying of materials.
[0082] A bracket 104 is fixed to the periphery of the deodorization and odor removal cylinder 101, an air outlet pipe 105 is fixed to the top of the deodorization and odor removal cylinder 101, a blower 106 is fixed to the bottom of one side of the bracket 104, an air inlet pipe 107 is fixedly connected to the air outlet of the blower 106, and one end of the air inlet pipe 107 is fixedly connected to one side of the waste heat recovery cylinder 103.
[0083] A support 113 is fixed to the top of the deodorization and odor removal cylinder 101. A motor 114 is fixed to the top surface of the support 113. One end of the output shaft of the motor 114 passes through the first inclined tube 202 and the top of the deodorization and odor removal cylinder 101 and is fixed with a rotating shaft 115. A first carbon adsorption cylinder 116 is sleeved and fixed to the circumference of the rotating shaft 115. A second carbon adsorption cylinder 117 is fixed to the inner wall of the deodorization and odor removal cylinder 101.
[0084] Among them, such as Figure 1 As shown, a platform 204 is fixed to the bottom periphery of the spiral elevator 2, and several support legs 205 are fixed to the bottom of the platform 204.
[0085] Among them, such as Figure 1-2 As shown, the bracket 104 includes a fixed platform 108, which is fixed to the side of the deodorization and odor removal cylinder 101. The bottom of the fixed platform 108 is rectangular and has several columns 109 fixed on it.
[0086] Among them, such as Figure 1-2 As shown, a heater 110 is fixed to the periphery of the heating cylinder 102, and the heating end of the heater 110 is located inside the heating cylinder 102.
[0087] Among them, such as Figure 1-2 As shown, the bottom of the waste heat recovery cylinder 103 is fixedly connected to the discharge pipe 111, and the discharge pipe 111 is equipped with a flow valve 112.
[0088] Among them, the deodorization and odor removal cylinder 101, the waste heat recovery cylinder 103, the heating cylinder 102, the first inclined tube 202, the second inclined tube 203 and the two sides of the spiral elevator are all wrapped and fixed with rock wool layers, and steel sleeves are fixed to the outside of the rock wool layers.
[0089] Among them, such as Figure 2 As shown, the connection end of the first inclined tube 202 and the deodorization cylinder 101 is concentrically arranged with the deodorization cylinder 101. The rotating shaft 115 is located at the axis of the first inclined tube 202 and the deodorization cylinder 101, and the diameter of the rotating shaft 115 is half the diameter of the first inclined tube 202.
[0090] The working principle of the above-mentioned deodorization and deodorization machine is as follows: the material is discharged into the screw conveyor 2 through the feed pipe 201. The operation of the screw conveyor 2 drives the material at the bottom of the screw conveyor 2 to be spirally conveyed upward. The material lifted by the screw conveyor 2 gradually fills the waste heat recovery cylinder 103, the heating cylinder 102 and the deodorization and deodorization cylinder 101 from bottom to top through the first inclined pipe 202. The motor 114 drives the rotating shaft 115 and the first carbon adsorption cylinder 116 to rotate, and works with the second carbon adsorption cylinder 117 to achieve efficient deodorization. The discharge pipe 111 is controlled to discharge the material evenly through the flow valve 112. At the same time, the blower 106 blows air into the waste heat recovery cylinder 103. Some of the gas passes through the heating cylinder 102 and carries a large amount of heat from the waste heat recovery cylinder 103 and the heating cylinder 102 to the deodorization and deodorization cylinder 101, which can perform deodorization and deodorization. Meanwhile, another part of the gas carries the heated material and flows back to the bottom of the screw conveyor 2 through the second inclined pipe 203 in a certain proportion.
[0091] Although preferred embodiments of the present invention have been described in detail above, it should be clearly understood that various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A method for preparing a low-odor glass fiber reinforced nylon modified material, characterized in that: Prepared using raw materials with the following weight fractions: PA6 sections 60-78% 20-32% glass fiber Additives 0.1-0.2%, Carbon powder 1.0-2.0%, The sum of the weight fractions of the above four raw materials is 100%. The carbon powder serves as a black masterbatch and an odor adsorbent. The preparation method includes the following steps: (1) Immerse the glass fiber in an aminosilane coupling agent dispersion; (2) Mix PA6 chips, additives and carbon powder and add them to the polymerization high pressure reactor from the main material port. Filter the dispersion system of step (1), take the filter residue and add it to the polymerization high pressure reactor. At the same time, add deionized water accounting for 0.8-2% of PA6 content. Seal the reactor and pressurize the reaction for 3-7 hours. The reaction pressure is 6-12 MPa and the reaction temperature is 200-280℃. After the reaction is completed, discharge the material and dry it at 60-80℃ for more than 2 hours. (3) Transfer the reactants from step (2) to another polymerization reactor, evacuate and reduce the pressure to 1×10⁻⁶. 3 After the Pa is below, start heating and set the reaction temperature to 160-220℃. Turn on the cooling to maintain the reaction temperature and react for 8-12 hours. Then, discharge the melt through the screw and extrude it through the wire casting head. Cool and pelletize it in the cooling bath. The pellets are then extracted and improved at a high temperature of 80℃-100℃. (4) Dry the granules from step (3) in a vacuum oven, feed the material into a twin-screw extruder, turn on the vacuum pump of the extruder, set a film forming device at the top of the barrel, and set the temperature of the twin-screw extruder as follows: Zone 1: 250-270℃, Zone 2: 250-270℃, Zone 3: 240-260℃, Zone 4: 230-250℃, Zone 5: 220-240℃, Zone 6: 220-240℃, Zone 7: 220-240℃, Zone 8: 220-240℃, Zone 9: 230-250℃; (5) After the material is discharged from the extruder, it enters a cooling water tank at 20-30℃ and then enters a pelletizer at a speed of 700-1200r / min. After being screened by a vibrating screen, it undergoes high-temperature steam extraction at 80℃-100℃. (6) Drying and removing the devolatilization from the granules.
2. The method for preparing the low-odor glass fiber reinforced nylon modified material according to claim 1, characterized in that: The moisture content of PA6 in the raw material is 0.25-0.5%.
3. The method for preparing the low-odor glass fiber reinforced nylon modified material according to claim 1, characterized in that: The length of the glass fiber in the raw material is 3.0±1.0 mm.
4. The method for preparing the low-odor glass fiber reinforced nylon modified material according to claim 1, characterized in that: The additives are selected from one or more of antioxidants, lubricants, and catalysts.
5. The method for preparing the low-odor glass fiber reinforced nylon modified material according to claim 1, characterized in that: In step (1), the aminosilane coupling agent is aminoethylaminopropyltrimethoxysilane or KH550 silane coupling agent.
6. The method for preparing the low-odor glass fiber reinforced nylon modified material according to claim 1, characterized in that: Granular material drying and deodorization are accomplished by a drying and deodorization deodorization machine, which includes a deodorization deodorization device (1), the deodorization deodorization device (1) including a deodorization deodorization cylinder (101), the bottom of the deodorization deodorization cylinder (101) is fixedly connected to a heating cylinder (102), the bottom of the heating cylinder (102) is fixedly connected to a waste heat recovery cylinder (103), characterized in that: it also includes a screw conveyor (2); the bottom peripheral side of the screw conveyor (2) is fixedly connected to a feed pipe (201), the top peripheral side of the screw conveyor (2) and the top of the deodorization deodorization cylinder (101) are fixedly connected to a first inclined pipe (202), the peripheral side of the waste heat recovery cylinder (103) and the bottom peripheral side of the screw conveyor (2) are fixedly connected to a second inclined pipe (203); the peripheral side of the deodorization deodorization cylinder (101 ... feed pipe (201) is fixedly connected to a feed pipe (201), the feed pipe (202) is fixedly connected to a feed pipe (202), the feed pipe (202) is fixedly connected to a feed pipe (203), the feed pipe (202) is fixedly connected to a feed pipe (203), the feed pipe (202) is fixedly connected to a feed pipe (202), the feed pipe (202) is fixedly connected to a feed pipe (202), the feed pipe A support (104) is fixed, an air outlet pipe (105) is fixed at the top of the deodorization and odor removal cylinder (101), a blower (106) is fixed at the bottom of one side of the support (104), an air outlet pipe (107) is fixedly connected to the air outlet of the blower (106), and one end of the air outlet pipe (107) is fixedly connected to one side of the waste heat recovery cylinder (103); a support (113) is fixed at the top of the deodorization and odor removal cylinder (101), a motor (114) is fixed on the top surface of the support (113), one end of the output shaft of the motor (114) passes through the first inclined tube (202) and the top of the deodorization and odor removal cylinder (101) and is fixed with a rotating shaft (115), a first carbon adsorption cylinder (116) is sleeved and fixed on the circumferential side of the rotating shaft (115), and a second carbon adsorption cylinder (117) is fixed on the inner wall of the deodorization and odor removal cylinder (101).
7. The method for producing a low-odor glass fiber reinforced nylon modified material according to claim 6, characterized in that: The bottom periphery of the spiral elevator (2) is fixed with a platform (204), and a number of legs (205) are fixed at the bottom of the platform (204).
8. The method for producing a low-odor glass fiber reinforced nylon modified material according to claim 6, characterized in that: The bracket (104) includes a fixed platform (108), which is fixed to the periphery of the deodorization and odor removal cylinder (101). The bottom of the fixed platform (108) is rectangular and has several columns (109) fixed on it.
9. The method for producing a low-odor glass fiber reinforced nylon modified material according to claim 6, characterized in that: A heater (110) is fixed on the periphery of the heating cylinder (102), and the heating end of the heater (110) is located inside the heating cylinder (102); a discharge pipe (111) is fixedly connected to the bottom of the waste heat recovery cylinder (103), and a flow valve (112) is provided on the discharge pipe (111).
Citation Information
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