CN113789051B - Glass fiber reinforced nylon composite material and preparation method thereof - Google Patents
Glass fiber reinforced nylon composite material and preparation method thereof Download PDFInfo
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- CN113789051B CN113789051B CN202111155835.0A CN202111155835A CN113789051B CN 113789051 B CN113789051 B CN 113789051B CN 202111155835 A CN202111155835 A CN 202111155835A CN 113789051 B CN113789051 B CN 113789051B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a glass fiber reinforced nylon composite material and a preparation method thereof, wherein the glass fiber reinforced nylon composite material comprises the following components in parts by weight: 110-130 parts of nylon 66; 50-80 parts of long glass fibers (diameter 10 μm); 15-25 parts of a toughening agent; 10-15 parts of flame retardant; the nylon 66 is prepared from hexamethylenediamine and adipic acid into an aqueous solution of nylon 66 salt, and the nylon 66 is prepared through polycondensation reaction. The invention controls the screw rotating speed of the homodromous double screw extruder, can uniformly disperse glass fibers in nylon 66, obtain a modified nylon composite material with high quality of flame retardant and extruded continuous strips, further improves the flame retardance and mechanical properties of the modified nylon composite material, and in addition, the invention achieves the purposes of ensuring constant cooling water volume in a water tank, ensuring constant cooling residence time and strong cooling effect, and ensuring the quality of the modified nylon composite material.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a glass fiber reinforced nylon composite material and a preparation method thereof.
Background
The reinforced nylon is prepared by adding glass fiber, toughening agent and other blending materials into nylon, and the results show that the tensile strength and bending strength of the material are greatly improved along with the increase of the content of the glass fiber, the impact strength is more complicated, the toughening agent is added, the toughness of the material is greatly improved, 30-35% of the glass fiber and 8-12% of the toughening agent are added, and the comprehensive mechanical property of the material is optimal. Has excellent wear resistance, heat resistance and electrical property, high mechanical strength, self-extinguishment and good dimensional stability, the method is widely applied to automobile industry products, textile products, pump impellers and primary precision engineering parts;
the performance of the nylon composite material, such as flame-retardant nylon, corrosion-resistant nylon and the like, can be changed by adding the modifier into the nylon, the flame-retardant performance of the flame-retardant nylon is closely related to the temperature in the preparation process, as the nylon and the glass fiber are blended in the co-rotating twin-screw extruder, the screw rotating speed of the co-rotating twin-screw extruder is not accurately qualitative, the glass fiber is not uniformly dispersed in the nylon, the mechanical strength is often difficult to achieve the expected effect, in the basic cooling process, the water volume in the cooling tank is reduced due to the generated water vapor along with the rise of the water temperature in the cooling tank, the constancy of the water volume of the cooling tank cannot be realized in a mechanical mode at present, the retention time of the strip-shaped modified nylon in the cooling tank is directly shortened, and the cooling effect is poor.
Disclosure of Invention
The invention aims to provide a glass fiber reinforced nylon composite material and a preparation method thereof, which at least solve the problems that the flame retardance and the mechanical property of flame retardant nylon cannot be expected directly due to the uncertainty of the screw rotating speed of a co-rotating double screw extruder when the modified nylon in the prior art is blended, and the extruded modified nylon has short cooling time and poor cooling effect.
In order to achieve the above purpose, the present invention provides the following technical solutions: the glass fiber reinforced nylon composite material comprises the following components in parts by weight:
the nylon 66 is prepared into nylon 66 salt water solution by hexamethylenediamine and adipic acid, and nylon 66 is prepared by polycondensation reaction;
the preparation method comprises the following steps:
(1) The nylon 66 and the toughening agent are put into an open mill for blending grafting modification, the blending time is controlled to be 20-30min, and the temperature is controlled to be 250-300 ℃ to obtain toughened nylon 66;
(2) Adding a flame retardant into the toughened nylon 66 to obtain modified nylon 66;
(3) Immersing the long glass fiber in a silane coupling agent KH-550 for 5-10min, baking at 110-120 ℃ for 40min, and drying and dehydrating for later use;
(4) The treated long glass fiber and the modified nylon 66 are put into a co-rotating double-screw extruder to be mixed, so as to obtain a modified nylon composite material, and the modified nylon composite material is extruded in a strip shape by the co-rotating double-screw extruder;
(5) The strip-shaped modified nylon composite material is cooled by cooling equipment, dried and granulated by a granulator to form modified nylon composite material particles.
Preferably, the coupling agent is a vinyl elastomer, and the flame retardant is halogen-free ethyl phosphate oligomer dihydric alcohol.
Preferably, the mass fraction of the glass fiber is 30% -33%.
Preferably, in the step (4), the screw speed of the co-rotating twin-screw extruder is controlled to be 400rpm, and the temperature is 270 ℃.
Preferably, the cooling apparatus includes: a valve is arranged at the bottom end of the front side of the water tank; the first rollers are two in number and are respectively rotatably arranged at the left side and the right side of the inner cavity of the water tank; the number of the second rollers is two, and the second rollers are respectively rotatably arranged at the left end and the right end of the top of the water tank; the water surface regulating and controlling mechanism is arranged on the left inner wall of the water tank.
Preferably, the water surface control mechanism includes: the shell is arranged on the left inner wall of the water tank, a through hole is formed in the bottom end of the shell, and the inner cavity is circular; the rotating shaft is rotatably arranged at the center of the inner cavity of the shell, and the right end of the rotating shaft extends out of the right side wall of the shell; the valve plate is arranged on the outer wall of the rotating shaft and is positioned in the inner cavity of the shell, and a diversion hole is formed in the side wall of the valve plate; and the bent pipe is arranged on the front side of the shell and extends out of the front side surface of the water tank.
The glass fiber reinforced nylon composite material and the preparation method thereof provided by the invention have the beneficial effects that:
1. according to the invention, through mixing of the flame retardant and control of the screw speed of the co-rotating double screw extruder, glass fibers can be uniformly dispersed in nylon 66, so that a modified nylon composite material with high flame retardant quality and continuous extrusion is obtained, and the flame retardance and mechanical properties of the modified nylon composite material are further improved;
2. according to the invention, the strip-shaped modified nylon composite material can be soaked in the water tank through the cooperation of the first roller and the second roller, cooling is realized, the floating ball moves along with the height of the liquid level of cooling water, the rotating shaft can drive the valve plate to rotate, the on/off of the guide hole on the bent pipe is realized, the constant volume of cooling water in the water tank is realized, the constant cooling residence time is ensured, the cooling effect is strong, and the quality of the modified nylon composite material is ensured.
Drawings
FIG. 1 is a graph of the relationship between the rotational speed of a screw and the average length of glass fibers according to the present invention;
FIG. 2 is a graph of the relationship between screw speed and material impact properties of the present invention;
FIG. 3 is a schematic view of a cooling apparatus according to the present invention;
FIG. 4 is a schematic view of a water surface control mechanism according to the present invention;
FIG. 5 is a right side cross-sectional view of the water surface control mechanism of the present invention.
In the figure: 1. the water tank, 2, the first roller, 3, the second roller, 4, the water surface regulating mechanism, 41, the shell, 42, the rotating shaft, 43, the valve plate, 44, the diversion hole, 45, the bent pipe, 46, the supporting rod, 47 and the floating ball.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-5, the present invention provides a technical solution: the glass fiber reinforced nylon composite material comprises the following components in parts by weight:
nylon 66 is prepared from hexamethylenediamine and adipic acid into nylon 66 salt water solution, and nylon 66 is prepared through polycondensation reaction;
the preparation method comprises the following steps:
(1) Nylon 66 and a toughening agent are put into an open mill for blending grafting modification, the blending time is controlled to be 20-30min, the temperature is 265 ℃, the toughened nylon 66 is obtained, the blending grafting belongs to copolymerization reaction, the dispersion and interface conditions of nylon 66 solution are improved, the viscosity is higher, and the blending effect with glass fiber is facilitated;
(2) Adding a flame retardant into the toughened nylon 66 to obtain modified nylon 66, and improving the flame retardant property of the material;
(3) Soaking long glass fiber in a silane coupling agent KH-550 for 5-10min, baking at 110-120 ℃ for 40min, drying and dehydrating for standby, hydrolyzing the silane coupling agent to generate a compound containing active hydroxyl, wherein the active hydroxyl can perform condensation reaction with hydroxyl in the glass fiber, silane and the glass fiber form a silica bond, thermal decomposition is avoided in the sintering process, and the silane coupling agent plays a role in connecting the glass fiber and nylon 66;
(4) The treated long glass fiber and the modified nylon 66 are put into a co-rotating twin-screw extruder to be mixed, so as to obtain a modified nylon composite material, and the modified nylon composite material is extruded in a strip shape by the co-rotating twin-screw extruder;
(5) The strip-shaped modified nylon composite material is cooled by cooling equipment, dried and granulated by a granulator to form modified nylon composite material particles.
As a preferable scheme, the toughening agent is vinyl elastomer and is subjected to copolymerization reaction with nylon 66, so that the purpose of improving the viscosity and fluidity of the nylon 66 solution is achieved, the flame retardant is halogen-free ethyl phosphate oligomer dihydric alcohol, and the modified nylon composite material does not generate toxic gas at high temperature or during combustion and does not cause harm to human bodies.
As a preferred solution, the mass fraction of the glass fiber is 30% -33%, and according to the research of the traditional reinforced nylon, the glass fiber has the best mechanical property during the period of the glass fiber.
As a preferable scheme, in the step (4), the screw rotating speed of the co-rotating double screw extruder is controlled at 400rpm, the temperature is 270 ℃, the glass fibers are prevented from being shortened due to the influence of shearing force caused by overhigh rotating speed, and the glass fibers are uniformly dispersed in nylon 66, so that the volatilization of the flame retardant caused by overhigh extruding temperature is prevented, and the extrusion breakage is avoided.
As the preferred scheme, still further, cooling arrangement includes basin 1, first cylinder 2, second cylinder 3 and surface of water regulation and control mechanism 4, the valve is installed to basin 1 front side bottom, basin 1 is used for storing cooling water, first cylinder 2 quantity is two, rotationally install in the inner chamber left and right sides of basin 1 respectively, through the cooperation of first cylinder 2 and second cylinder 3, can make the strip modified nylon composite who extrudes soak in cooling water, reach the refrigerated purpose, second cylinder 3 quantity is two, rotationally install in the top left and right sides both ends of basin 1 respectively, surface of water regulation and control mechanism 4 installs in the left inner wall of basin 1.
As a preferred scheme, further, the water surface regulating mechanism 4 includes a housing 41, a rotating shaft 42, a valve plate 43, a diversion hole 44, an elbow 45, a supporting rod 46 and a floating ball 47, the housing 41 is mounted on the left inner wall of the water tank 1, a through hole is formed at the bottom end of the housing 41, the inner cavity is circular, the valve plate 43 is convenient to rotate in the housing, the rotating shaft 42 is rotatably mounted on the central position of the inner cavity of the housing 41, the right end of the rotating shaft 42 extends out of the right side wall of the housing 41, the valve plate 43 is mounted on the outer wall of the rotating shaft 42 and is positioned in the inner cavity of the housing 41, the rotation of the valve plate 43 can realize the on and off between the diversion hole 44 and the elbow 45, the diversion hole 44 is formed in the side wall of the valve plate 43, the elbow 45 is mounted on the front side of the housing 41, the elbow 45 extends out of the front surface of the water tank 1, one end of the supporting rod 46 is mounted on the right end of the outer wall of the rotating shaft 42, the floating ball 47 is mounted on the other end of the supporting rod 46, the floating ball 47 can change along with the lifting of the liquid surface of cooling water by utilizing the floating ball 47, and further controlling the rotation of the rotating shaft 42.
In order to explore the influence of the processing temperature on the material performance, the traditional processing temperature is used as a basis, and the temperature of 260 ℃, 270 ℃ and 280 ℃ are respectively set for the same-direction double-screw extruder extrusion;
in the extrusion process at 260 ℃, the die head of the extruder is easy to be blocked, the strip breakage phenomenon does not occur at 270 ℃, the surface of the strip is smooth, the extruded strip is broken frequently at 280 ℃, the glass fiber is seriously exposed, and a large amount of white smoke appears at the die head due to the thermal decomposition of the flame retardant, so that the optimal processing temperature is 270 ℃.
The screw speeds of the co-rotating twin-screw extruder are adjusted to be respectively as follows under the process of processing temperature of 270 ℃ and feeding speed of 40 Kg/hr: 200. 300, 400, 500 and 600rpm to study the influence of shearing on the material performance, after the extruded particles are calcined at a high temperature of 650 ℃ for 4 hours, the glass fibers are scattered and tiled under an optical microscope, the length and the number of each glass fiber are recorded through VDM1.5 software, the sum of each length of the total number of the detected glass fibers is divided by the total number of the glass fibers, and the number average length of the glass fibers is obtained, as shown in an attached figure 1 of the specification;
taking injection molding of an injection molding machine as a standard for impact test, and testing notch impact of the co-rotating double-screw extruder at different rotating speeds by an impact tester, wherein the notch impact is shown in an attached figure 2 of the specification;
as can be seen from figures 1 and 2 of the description, when the screw speed exceeds 400rpm, the length of the glass fibers decreases dramatically, as high speeds result in higher shear, increased likelihood of shear fracture of the glass fibers, and localized temperature increases in the barrel of the co-rotating twin screw extruder, causing partial degradation of the matrix resin. With the increase of the shearing, the dispersion degree of the glass fiber is gradually increased, the impact performance of the material is gradually increased, but with the increase of the shearing again, the reduction of the length of the glass fiber and the reduction of the resin performance can lead to the rapid reduction of the overall impact performance of the material;
in summary, for glass fiber reinforced nylon, a certain length of glass fiber and a good matrix binding force can greatly improve the mechanical properties of the material, so that the optimal point of the properties can be reached when the screw speed is 400 rpm.
The detailed connection means are known in the art, and the following mainly describes the working principle and process, and the specific work is as follows.
Compared with the traditional phosphorus-containing flame retardant, the flame retardant is nontoxic, meets the increasingly strict requirements of environmental protection and flame retardation regulations, can improve the flame retardant property of the modified nylon, adopts the screw rotation speed of 400rpm of a homodromous double screw extruder, can uniformly disperse glass fibers in nylon 66, prevents the glass fibers from shortening due to overlarge screw shearing force, ensures the strength of the modified nylon, ensures the most proper extrusion temperature at 270 ℃, easily causes the blockage of a die head of the homodromous double screw extruder due to the overlow temperature, avoids the thermal decomposition and volatilization of the flame retardant, ensures the content of the flame retardant in the modified nylon, and thus obtains the modified nylon with excellent flame retardant property and high mechanical strength;
when the extruded strip-shaped modified nylon is required to be cooled, the bent pipe 45 is connected with an external water tank through a water pipe, so that the strip-shaped modified nylon passes through the top of the second roller 3 and passes through the bottom of the first roller, the strip-shaped modified nylon can be soaked in cooling water in the water tank 1, the strip-shaped modified nylon is cooled along with the cooling water absorbing heat of the strip-shaped modified nylon, the cooling water after absorbing heat forms vapor for evaporation, the cooling water volume in the water tank 1 is reduced, the floating ball 47 is lowered, the supporting rod 46 drives the rotating shaft 42 to rotate, the valve plate 43 is driven to rotate, when the diversion hole 44 is aligned with the bent pipe 45, the cooling water can be introduced into the water tank 1 through the diversion hole 44, the supplement of the cooling water is realized, the floating ball 47 is gradually raised along with the rise of the liquid level of the cooling water, the valve plate 43 rotates, and when the valve plate 43 blocks the bent pipe 45, the cooling water is stopped from being added in the water tank 1, and the automatic addition of the cooling water in the water tank 1 is realized;
in conclusion, the modified nylon has flame retardant property, the mechanical property is optimal, the volume of cooling water in the water tank 1 is constant, the cooling effect of the strip-shaped modified nylon is ensured, and the quality of the modified nylon is further ensured.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The preparation method of the glass fiber reinforced nylon composite material is characterized by comprising the following components in parts by weight:
the nylon 66 is prepared into nylon 66 salt water solution by hexamethylenediamine and adipic acid, and nylon 66 is prepared by polycondensation reaction;
the preparation method comprises the following steps:
(1) The nylon 66 and the toughening agent are put into an open mill for blending grafting modification, the blending time is controlled to be 20-30min, and the temperature is controlled to be 250-300 ℃ to obtain toughened nylon 66;
(2) Adding a flame retardant into the toughened nylon 66 to obtain modified nylon 66;
(3) Immersing the long glass fiber in a silane coupling agent KH-550 for 5-10min, baking at 110-120 ℃ for 40min, and drying and dehydrating for later use;
(4) The treated long glass fiber and the modified nylon 66 are put into a co-rotating double-screw extruder to be mixed, so as to obtain a modified nylon composite material, and the modified nylon composite material is extruded in a strip shape by the co-rotating double-screw extruder;
(5) The strip-shaped modified nylon composite material is cooled by cooling equipment, dried and granulated by a granulator to form modified nylon composite material particles;
the cooling apparatus includes:
a valve is arranged at the bottom end of the front side of the water tank (1);
the number of the first rollers (2) is two, and the first rollers are respectively rotatably arranged at the left side and the right side of the inner cavity of the water tank (1);
the number of the second rollers (3) is two, and the second rollers are respectively rotatably arranged at the left end and the right end of the top of the water tank (1);
the water surface regulating mechanism (4) is arranged on the left inner wall of the water tank (1);
the water surface regulating mechanism (4) comprises:
the shell (41) is arranged on the left inner wall of the water tank (1), a through hole is formed in the bottom end of the shell (41), and the inner cavity is circular;
the rotating shaft (42) is rotatably arranged at the center of the inner cavity of the shell (41), and the right end of the rotating shaft (42) extends out of the right side wall of the shell (41);
the valve plate (43) is arranged on the outer wall of the rotating shaft (42) and is positioned in the inner cavity of the shell (41), and a diversion hole (44) is formed in the side wall of the valve plate (43);
an elbow pipe (45) mounted on the front side of the housing (41), the elbow pipe (45) extending out of the front surface of the water tank (1);
one end of the supporting rod (46) is arranged at the right end of the outer wall of the rotating shaft (42);
and a floating ball (47) which is arranged at the other end of the supporting rod (46).
2. The method for preparing the glass fiber reinforced nylon composite according to claim 1, wherein the method comprises the following steps: the flame retardant is halogen-free ethyl phosphate oligomer dihydric alcohol.
3. The method for preparing the glass fiber reinforced nylon composite according to claim 1, wherein the method comprises the following steps: the mass fraction of the glass fiber is 30% -33%.
4. The method for preparing the glass fiber reinforced nylon composite according to claim 1, wherein the method comprises the following steps: the screw speed of the co-rotating twin-screw extruder in the step (4) is controlled at 400rpm, and the temperature is 270 ℃.
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| CN100410324C (en) * | 2006-10-30 | 2008-08-13 | 东北林业大学 | Glass fibre reingorced no-halogen flame-retardant nylon 66 and its preparing method |
| JP2008043779A (en) * | 2007-09-21 | 2008-02-28 | Sharp Corp | Washing drying machine and control method thereof |
| CN206217147U (en) * | 2016-11-07 | 2017-06-06 | 荆门市银珠塑化有限公司 | A kind of cooling device of plastic strip |
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