CN105331055B - PBT composite material used for NMT forming and preparation method thereof - Google Patents
PBT composite material used for NMT forming and preparation method thereof Download PDFInfo
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- CN105331055B CN105331055B CN201510704753.5A CN201510704753A CN105331055B CN 105331055 B CN105331055 B CN 105331055B CN 201510704753 A CN201510704753 A CN 201510704753A CN 105331055 B CN105331055 B CN 105331055B
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Abstract
The invention relates to a PBT composite material used for NMT forming and a preparation method thereof. The PBT composite material used for NMT forming is characterized by being prepared from, by mass, 100 parts of polybutylene terephthalate, 10-15 parts of flexibilizers, 30-40 parts of reinforcing agents, 3-5 parts of lubricating agents, 5-8 parts of compatilizers, 0.2-0.8 part of nano materials, 0.5-1 part of antioxidants and 0.5-1 part of coupling agents. The nano materials are prepared from at least one of nano alumina, nano magnesia and nano iron oxide. The reinforcing agents are prepared from glass fibers. The PBT composite material used for NMT forming can be applied to NMT forming.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to for the PBT composite of NMT molding, its preparation
Method.
Background technology
NMT (Nano Molding Technology) be by metal integrated with plastics nanometer forming technique, earliest by
Japanese great achievement plastics Co., Ltd. (Taiseiplas) exploitation, can be by the metals such as aluminum, magnesium, rustless steel, titanium and hard resin one
Chemical conversion type.NMT forming technique large-scale applications is thin, light, portable 3C Product at present, such as outside notebook computer shell, projector
Shell, phone housing, MP3 player etc..NMT forming technique core concepts are to combine metal, plastics, replace what is commonly used at present
Embedded injection, zinc-aluminium, magnalium die casting, there is provided a kind of that there is price advantage, high performance modeling gold integrated product.
The treatment process of NMT includes flow process as follows：The metal for needing to combine is carried out into base extraction, acid treatment, T
Liquid (ester propylhomoserin) process, cleaned up with water again after be dried, be molded.Metal surface Jing after processing, will be in metal watch
Face forms countless apertures and is about 20nm micropores, that is to say, that may be considered and is being formed on the metal surface after process
Many small concaveconvex structures, the resin of injection are entered in these concaveconvex structures, produce anchoring effect.Meanwhile, when resin is noted
During the metal surface being mapped to after processing, the resin containing ester group will occur the reaction of ester amine with T liquid, so as to combine closely one
Rise.
At present, the metal material that can be used for NMT molding is concentrated mainly on aluminium, magnesium material, at the same also have copper, rustless steel,
Titanium, ferrum, red copper various metals are bondd.The resin that can be used also has PBT, PPS, nylon 6, nylon66 fiber.Saturated linear half hitch
Crystalline substance polyester PBT has excellent mechanical property, good fatigue durability, preferable impact flexibility, relatively low coefficient of friction, good
Good thermostability and preferable moulding processability.
In recent years, fiberglass reinforced modified PBT material being adopted domestic and international research worker more, PBT material not only can be lifted
Physical and mechanical propertiess, while also have in terms of solving the endurance life of PBT material, weatherability, frictional behaviour
Really.But glass fiber reinforcement PBT material still has weak point, that is, when being molded big part product or thin-walled parts, have larger
Warpage occurs, and this not only affects the outward appearance of product, while affecting the service life of modified PBT material.Retrieve substantial amounts of patent text
The research paper offered and publish, there is not yet being applied to the research report of the PBT material of NMT molding, particularly has no employing
Polybutylene terephthalate (PBT) (PBT) is raw material, adds ethylene-octene block copolymer OBC, nano-sized iron oxide, nano oxygen
Change magnesium or nano aluminium oxide, flat alkali-free glass fibre and chopped alkali-free glass fibre, preparation can be used for the poly- to stupid of NMT molding
Dioctyl phthalate butanediol ester (PBT) composite.
The content of the invention
Based on this, it is necessary to provide a kind of PBT composite that can apply to NMT molding and preparation method thereof.
A kind of PBT composite for NMT molding, according to mass fraction meter, including following components：
Wherein, at least one of the nano material in nano aluminium oxide, nano magnesia and nano-sized iron oxide, institute
Reinforcing agent is stated for glass fibre.
Wherein in one embodiment, the toughener be ethylene-octene block copolymer, octene in the toughener
Mass content is 47%～53%.
Wherein in one embodiment, the reinforcing agent is in flat alkali-free glass fibre and chopped alkali-free glass fibre
At least one.
Wherein in one embodiment, the lubricant is polysiloxanes.
Wherein in one embodiment, the compatilizer is common for ethylene oxidic ester, ethylene and methyl ester acrylic acid methyl ester. ternary
Polymers.
Wherein in one embodiment, the coupling agent is silane coupler.
Wherein in one embodiment, the particle diameter of the nano material is 104nm～157nm.
Wherein in one embodiment, the antioxidant is phenolic antioxidant.
A kind of preparation method of the PBT composite for NMT molding, comprises the steps：
According to mass fraction meter, following raw material is weighed：100 parts of polybutylene terephthalate (PBT), 10～15 parts of toughener,
30～40 parts of reinforcing agent, 3～5 parts of lubricant, 5～8 parts of compatilizer, 0.2～0.8 part of nano material, 0.5～1 part of antioxidant and
0.5～1.0 part of coupling agent, wherein, the nano material in nano aluminium oxide, nano magnesia and the nano-sized iron oxide extremely
Few one kind, the reinforcing agent are glass fibre；
In the coupling agent 1%～3% and ethanol are hybridly prepared into into the first solution, by the nano material with it is described
First solution high-speed stirred at 62 DEG C～86 DEG C obtains the first material；
The remaining coupling agent and ethanol are hybridly prepared into into the second solution, by the reinforcing agent and second solution
At 57 DEG C～76 DEG C, stirring at low speed obtains the second material；
By the polybutylene terephthalate (PBT), the toughener, the lubricant, the compatilizer and the antioxygen
Compound is obtained after agent mixed at high speed, is added the compound as the first material in extruder, first material passes through
Main feed system is added, the second material is added by side feed system, and pelletize after extrusion obtains being combined for the PBT of NMT molding
Material.
Wherein in one embodiment, in first solution and in second solution, the coupling agent and the second
The mass ratio of alcohol is 1～3：2.3～7.
The above-mentioned PBT composite for NMT molding is by adding 10 in 100 parts of polybutylene terephthalate (PBT)
Part～15 parts of glass fibre as reinforcing agent, add 0.2～0.8 part of nano material to be compounded, significantly can reduce
For the linear expansion coefficient of the PBT composite of NMT molding, so as to metal base in terms of linear expansion coefficient with compared with
Good matching, effectively solves the problems, such as that the two is peeling-off at reference to section, so as to can be widely applied to NMT into
Type.
Specific embodiment
Further is made to PBT composite for NMT molding and preparation method thereof mainly in combination with specific embodiment below
Detailed description.
The PBT composite for NMT molding of one embodiment, according to mass fraction meter, including following components：
Wherein, at least one of the nano material in nano aluminium oxide, nano magnesia and nano-sized iron oxide, reinforcing agent
For glass fibre.
Polybutylene terephthalate (PBT) (PBT) is primary raw material.Preferably, PBT resin intrinsic viscosity be 1.15～
1.18dL/g, density are 1.31～1.33g/cm3, 223～227 DEG C of fusing point, quality 27～29g/10min of melt flow rate (MFR),
Tensile strength 55.2MPa, bending strength 81.7MPa.
Preferably, toughener be ethylene-octene block copolymer, in toughener the mass content of octene be 47%～
53%.It is further preferred that toughener quality 0.482～0.882g/10min of melt flow rate (MFR).Toughener is preferably DOWization
At least one in the INFUSE 9000 and INFUSE 9007 of company
Preferably, at least one of the reinforcing agent in flat alkali-free glass fibre and chopped alkali-free glass fibre.Specifically
, the aspect ratio of flat alkali-free glass fibre is 4：1, length is 3～6 millimeters；A diameter of the 9～13 of chopped alkali-free glass fibre
Micron, length are 3～6 millimeters.
Preferably, lubricant is polysiloxanes.Preferably Wa Ke companies of the Germany trade mark is PA445200 watt gram of silicone.
Preferably, compatilizer is ethylene oxidic ester, ethylene and methyl ester acrylic acid methyl ester. terpolymer.It is more preferably French
The product of Arkema, the trade mark are AX-8900.
Preferably, coupling agent is silane coupler.More preferably German BASF TU169 glycidyl ether oxygen propyl front threes
TMOS coupling agent.
Preferably, antioxidant is phenolic antioxidant.More preferably 1010 antioxidant of BASF IRGANOX
Preferably, the particle diameter of nano material is 104nm～157nm.
The above-mentioned PBT composite for NMT molding has advantages below：
(1), using ethylene oxidic ester, ethylene and methyl ester acrylic acid methyl ester. terpolymer.
As compatilizer, the acrylic acid methyl ester. chain in ethylene oxidic ester, ethylene and methyl ester acrylic acid methyl ester. terpolymer
Section during melting extrusion can with polybutylene terephthalate (PBT) occur ester exchange reaction, while with simple glass fiber
And hydroxyl the reacting property increase-volume on flat glass fiber surface, to realize simple glass fiber and flat glass fiber poly- right
It is dispersed in benzene dicarboxylic acid butanediol ester, so as to effectively improve the resistance to warping energy of composite, improve composite
Warpage issues, can significantly improve the notch impact strength of PBT material, the compatibility, mobility, crystallization rate, surface light
Pool etc..
(2), the glass fibre by adding 10 parts～15 parts in 100 parts of polybutylene terephthalate (PBT) is used as increasing
Strong agent, adds 0.2～0.8 part of nano material to be compounded, can significantly reduce the PBT composite for NMT molding
Linear expansion coefficient, so as to metal base in terms of linear expansion coefficient have preferable matching, effectively solve
The two peeling-off problem at reference to section, so as to can be widely applied to NMT molding.
The preparation method of the above-mentioned PBT composite for NMT molding, comprises the steps：
Step S110, according to mass fraction meter, weigh following raw material：100 parts of polybutylene terephthalate (PBT), toughener
10～15 parts, 30～40 parts of reinforcing agent, 3～5 parts of lubricant, 5～8 parts of compatilizer, 0.2～0.8 part of nano material, antioxidant
0.5～1 part, and 0.5～1.0 part of coupling agent, wherein, nano material is selected from nano aluminium oxide, nano magnesia and nano oxidized
At least one in ferrum, reinforcing agent are glass fibre.
Polybutylene terephthalate (PBT) (PBT) is primary raw material.Preferably, PBT resin intrinsic viscosity be 1.15～
1.18dL/g, density are 1.31～1.33g/cm3, 223～227 DEG C of fusing point, quality 27～29g/10min of melt flow rate (MFR),
Tensile strength 55.2MPa, bending strength 81.7MPa.
Preferably, toughener be ethylene-octene block copolymer, in toughener the mass content of octene be 47%～
53%.It is further preferred that toughener quality 0.482～0.882g/10min of melt flow rate (MFR).Toughener is preferably DOWization
At least one in the INFUSE 9000 and INFUSE 9007 of company
Preferably, at least one of the reinforcing agent in flat alkali-free glass fibre and chopped alkali-free glass fibre.Specifically
, the aspect ratio of flat alkali-free glass fibre is 4：1, length is 3～6 millimeters；A diameter of the 9～13 of chopped alkali-free glass fibre
Micron, length are 3～6 millimeters.
Preferably, lubricant is polysiloxanes.Preferably Wa Ke companies of the Germany trade mark is PA445200 watt gram of silicone.
Preferably, compatilizer is ethylene oxidic ester, ethylene and methyl ester acrylic acid methyl ester. terpolymer.It is more preferably French
The product of Arkema, the trade mark are AX-8900.
Preferably, coupling agent is silane coupler.More preferably German BASF TU169 glycidyl ether oxygen propyl front threes
TMOS coupling agent.
Preferably, antioxidant is phenolic antioxidant.More preferably 1010 antioxidant of BASF IRGANOX
Preferably, the particle diameter of nano material is 104nm～157nm.
Step S120,1%～3% in coupling agent and ethanol are hybridly prepared into into the first solution, by nano material and the
One solution high-speed stirred at 62 DEG C～86 DEG C obtains the first material.
Preferably, in the first solution, coupling agent is 1～3 with the mass ratio of ethanol：2.3～7.
Preferably, ethanol is dehydrated alcohol.
Preferably, coupling agent and ethanol are stirred at room temperature 2～3 minutes and make the first solution.
Preferably, the rotating speed of high-speed stirred is 800～1200rpm.
Preferably, the time of high-speed stirred is 8 minutes～10 minutes.
Preferably, nano material is placed in homogenizer, temperature setting is 62 DEG C～86 DEG C, and is set to low speed mould
Formula, adds mouth at the uniform velocity to add the first solution, charging to terminate rear high-speed stirred 8～10 minutes from liquid.Wherein, low-speed mode turn
Speed is 80～120rpm.
Step S130, remaining coupling agent and ethanol are hybridly prepared into into the second solution, reinforcing agent and the second solution are existed
At 57 DEG C～76 DEG C, stirring at low speed obtains the second material.
Preferably, in the second solution, coupling agent is 1～3 with the mass ratio of ethanol：2.3～7.
Preferably, ethanol is dehydrated alcohol.
Preferably, coupling agent and ethanol are stirred at room temperature 2～3 minutes and make the second solution.
Preferably, the rotating speed of stirring at low speed is 80～120rpm.
Preferably, the time of stirring at low speed is 6 minutes～8 minutes.
Preferably, reinforcing agent is placed in homogenizer, temperature setting is 57 DEG C～76 DEG C, and is set to low speed mould
Formula, adds mouth at the uniform velocity to add the first solution from liquid, and charging terminates rear stirring at low speed 6 minutes～8 minutes.
Step S140, by polybutylene terephthalate (PBT), toughener, lubricant, compatilizer and antioxidant mixed at high speed
After obtain compound, add mixture in extruder, the first material added by main feed system, while the second material passes through
Side feed system is added, and pelletize after extrusion obtains the PBT composite for NMT molding.
Preferably, first at 102 DEG C～118 DEG C, baking 1 hour～2 is little before mixing for polybutylene terephthalate (PBT)
When.
Preferably, polybutylene terephthalate (PBT), toughener, lubricant, compatilizer and antioxidant are placed in mixed at a high speed
Conjunction machine high speed mixes 5～7 minutes.
Preferably, extruder is double screw extruder.It is furthermore preferred that the design parameter of double screw extruder is, area's temperature
181～198 DEG C of degree, 218～229 DEG C of two area's temperature, 223～237 DEG C of three area's temperature, 235～247 DEG C of four area's temperature, five area's temperature
236～244 DEG C of degree, 219～232 DEG C of six area's temperature, 211～223 DEG C of seven area's temperature, 210～223 DEG C of eight area's temperature, nine area's temperature
Degree 210～225 DEG C, 238～246 DEG C of die temperature, the time of staying are 1～2 minute, and pressure is 5～7MPa.
The preparation method of the above-mentioned PBT composite for NMT molding is simple to operate, it is easy to industrialization；What is prepared is used for
The PBT composite of NMT molding has preferable matching in terms of linear expansion coefficient with metal base, effectively solves
The two peeling-off problem at reference to section, so as to can be widely applied to NMT molding.
It is below specific embodiment part：
Embodiment 1
The preparation process of the PBT composite for NMT molding of the present embodiment is as follows：
(1), according to the mass fraction, weigh the component in table 1：
Table 1
(2) nano material is placed in homogenizer, 1 part of silane coupler is placed in beaker in A, by silane coupled
Agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker A, while X minutes are stirred at room temperature so as to mix homogeneously；Start
Homogenizer, temperature setting are 70 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing and start fast mode, and high-speed stirred 8 minutes obtains the first material, wherein high
The rotating speed of speed stirring is 950rpm.
(3), glass fibre is placed in homogenizer, 1 part of silane coupler is placed in beaker in B, by silane idol
Connection agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker B, while being stirred at room temperature 8 minutes so as to mix homogeneously；Open
Dynamic homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silicon got ready in upper end liquid
Alkane coupling agent ethanol solution, coupling agent are added after finishing, stirring at low speed 3 minutes obtains the second material, and wherein stirring at low speed turns
Speed is 110rpm.
The preparation of step 3, PBT composite：
PBT resin is toasted into 4h at 120 DEG C, by dried PBT resin, toughener, lubricant, compatilizer, antioxygen
Agent etc. is placed in mixing X minutes in high-speed mixer, obtains mixture, feeds the mixture in double screw extruder, the first material
Added by main feed system, while the second material is added by side feed system, through melting extrusion, water-cooled, pelletizing, obtain
PBT composite.
Wherein, the design parameter of double screw extruder is, 185 DEG C of area's temperature, 195 DEG C of two area's temperature, three area's temperature 230
DEG C, 230 DEG C of four area's temperature, 220 DEG C of five area's temperature, 220 DEG C of six area's temperature, 220 DEG C of seven area's temperature, 220 DEG C of eight area's temperature, 9th area
230 DEG C of temperature, 235 DEG C of die temperature, the time of staying are 1 minute, and pressure is 4.2MPa.
Embodiment 2
The preparation process of the PBT composite for NMT molding of the present embodiment is as follows：
(1), according to the mass fraction, weigh the component in table 2：
Table 2
(2) nano material is placed in homogenizer, 1 part of silane coupler is placed in beaker in A, by silane coupled
Agent：Dehydrated alcohol is 1:7 weigh dehydrated alcohol is placed in beaker A, while being stirred at room temperature 2 minutes so as to mix homogeneously；Start high
Fast blender, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane idol got ready in upper end liquid
Connection agent ethanol solution, coupling agent are added after finishing and start fast mode, high-speed stirred minute, obtain the first material, its high speed
The rotating speed of stirring is 950rpm.
(3), glass fibre is placed in homogenizer, 1 part of silane coupler is placed in beaker in B, by silane idol
Connection agent：Dehydrated alcohol is 1：4 weigh dehydrated alcohol is placed in beaker B, while being stirred at room temperature 3 minutes so as to mix homogeneously；Start
Homogenizer, temperature setting are 67 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing, and stirring at low speed 3 minutes obtains the second material, the wherein rotating speed of stirring at low speed
For 95rpm.
The preparation of step 3, PBT composite：
PBT resin is toasted into 4h at 120 DEG C, by dried PBT resin, toughener, lubricant, compatilizer, antioxygen
Agent etc. is placed in high-speed mixer and mixes 9 minutes, obtains mixture, feeds the mixture in double screw extruder, the first material
Added by main feed system, while the second material is added by side feed system, through melting extrusion, water-cooled, pelletizing, obtain
PBT composite.
Wherein, the design parameter of double screw extruder is, 185 DEG C of area's temperature, 195 DEG C of two area's temperature, three area's temperature 230
DEG C, 230 DEG C of four area's temperature, 230 DEG C of five area's temperature, 220 DEG C of six area's temperature, 220 DEG C of seven area's temperature, 220 DEG C of eight area's temperature, 9th area
220 DEG C of temperature, 235 DEG C of die temperature, the time of staying are 1 minute, and pressure is 4.2MPa.
Embodiment 3
The preparation process of the PBT composite for NMT molding of the present embodiment is as follows：
(1), according to the mass fraction, weigh the component in table 3：
Table 3
(2) nano material is placed in homogenizer, 1 part of silane coupler is placed in beaker in A, by silane coupled
Agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker A, while being stirred at room temperature 3 minutes so as to mix homogeneously；Start
Homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing and start fast mode, and high-speed stirred 9 minutes obtains the first material, wherein high
The rotating speed of speed stirring is 950rpm.
(3), glass fibre is placed in homogenizer, 1 part of silane coupler is placed in beaker in B, by silane idol
Connection agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker B, while being stirred at room temperature 3 minutes so as to mix homogeneously；Open
Dynamic homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silicon got ready in upper end liquid
Alkane coupling agent ethanol solution, coupling agent are added after finishing, stirring at low speed 3 minutes obtains the second material, and wherein stirring at low speed turns
Speed is 90rpm.
The preparation of step 3, PBT composite：
PBT resin is toasted into 4h at 120 DEG C, by dried PBT resin, toughener, lubricant, compatilizer, antioxygen
Agent etc. is placed in high-speed mixer and mixes 9 minutes, obtains mixture, feeds the mixture in double screw extruder, the first material
Added by main feed system, while the second material is added by side feed system, through melting extrusion, water-cooled, pelletizing, obtain
PBT composite.
Wherein, the design parameter of double screw extruder is, 185 DEG C of area's temperature, 195 DEG C of two area's temperature, three area's temperature 230
DEG C, 230 DEG C of four area's temperature, 230 DEG C of five area's temperature, 220 DEG C of six area's temperature, 220 DEG C of seven area's temperature, 220 DEG C of eight area's temperature, 9th area
220 DEG C of temperature, 235 DEG C of die temperature, the time of staying are 1 minute, and pressure is 4.2MPa.
Embodiment 4
The preparation process of the PBT composite for NMT molding of the present embodiment is as follows：
(1), according to the mass fraction, weigh the component in table 4：
Table 4
(2) nano material is placed in homogenizer, 1 part of silane coupler is placed in beaker in A, by silane coupled
Agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker A, while being stirred at room temperature 9 minutes so as to mix homogeneously；Start
Homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing and start fast mode, and high-speed stirred 9 minutes obtains the first material, wherein high
The rotating speed of speed stirring is 900rpm.
(3), glass fibre is placed in homogenizer, 1 part of silane coupler is placed in beaker in B, by silane idol
Connection agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker B, while being stirred at room temperature 9 minutes so as to mix homogeneously；Open
Dynamic homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silicon got ready in upper end liquid
Alkane coupling agent ethanol solution, coupling agent are added after finishing, stirring at low speed 3 minutes obtains the second material, and wherein stirring at low speed turns
Speed is 95rpm.
The preparation of step 3, PBT composite：
PBT resin is toasted into 4h at 120 DEG C, by dried PBT resin, toughener, lubricant, compatilizer, antioxygen
Agent etc. is placed in high-speed mixer and mixes 9 minutes, obtains mixture, feeds the mixture in double screw extruder, the first material
Added by main feed system, while the second material is added by side feed system, through melting extrusion, water-cooled, pelletizing, obtain
PBT composite.
Wherein, the design parameter of double screw extruder is, 185 DEG C of area's temperature, 195 DEG C of two area's temperature, three area's temperature 225
DEG C, 230 DEG C of four area's temperature, 230 DEG C of five area's temperature, 220 DEG C of six area's temperature, 220 DEG C of seven area's temperature, 220 DEG C of eight area's temperature, 9th area
220 DEG C of temperature, 235 DEG C of die temperature, the time of staying are 1 minute, and pressure is 4.2MPa.
Embodiment 5
The preparation process of the PBT composite for NMT molding of the present embodiment is as follows：
(1), according to the mass fraction, weigh the component in table 5：
Table 5
(2) nano material is placed in homogenizer, 1 part of silane coupler is placed in beaker in A, by silane coupled
Agent：Dehydrated alcohol is 1:2.3 weigh dehydrated alcohol is placed in beaker A, while being stirred at room temperature 3 minutes so as to mix homogeneously；Start
Homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing and start fast mode, and high-speed stirred 9 minutes obtains the first material, wherein high
The rotating speed of speed stirring is 950rpm.
(3), glass fibre is placed in homogenizer, 1 part of silane coupler is placed in beaker in B, by silane idol
Connection agent：Dehydrated alcohol weighs dehydrated alcohol for 2.3 and is placed in beaker B, while being stirred at room temperature 3 minutes so as to mix homogeneously；Start
Homogenizer, temperature setting are 65 DEG C, are placed in low-speed mode, add mouth at the uniform velocity to add with the silane got ready in upper end liquid
Coupling agent ethanol solution, coupling agent are added after finishing, and stirring at low speed 3 minutes obtains the second material, the wherein rotating speed of stirring at low speed
For 90rpm.
The preparation of step 3, PBT composite：
PBT resin is toasted into 4h at 120 DEG C, by dried PBT resin, toughener, lubricant, compatilizer, antioxygen
Agent etc. is placed in high-speed mixer and mixes 9 minutes, obtains mixture, feeds the mixture in double screw extruder, the first material
Added by main feed system, while the second material is added by side feed system, through melting extrusion, water-cooled, pelletizing, obtain
PBT composite.
Wherein, the design parameter of double screw extruder is, 185 DEG C of area's temperature, 195 DEG C of two area's temperature, three area's temperature 210
DEG C, 230 DEG C of four area's temperature, 230 DEG C of five area's temperature, 230 DEG C of six area's temperature, 220 DEG C of seven area's temperature, 220 DEG C of eight area's temperature, 9th area
220 DEG C of temperature, 235 DEG C of die temperature, the time of staying are 1 minute, and pressure is 4.2MPa.
The PBT composite that embodiment 1～5 is obtained is made into standard sample test properties.Wherein, according to ISO527
Testing standard tests tensile strength and elongation at break；Bending strength and bending moduluses are tested according to ISO178 testing standards；Root
Notch impact strength (1/8 ") is tested according to ISO180 testing standards；Thermal distorsion temperature is tested according to ISO75 testing standards；By 1～5
The PBT composite for obtaining makes standard inserts detection metallo-plastic peel strength (MPa), and test result is shown in Table 6.
Table 6
As can be seen from Table 6：
1st, very well, stretch release is strong for its bonding to the metallic article Jing after T process of the result of 5 case study on implementation of the invention
Degree can reach more than 28Mpa.
2nd, Jing Comprehensive Correlations result understands that mass ratio is 1 in case study on implementation 3：3 chopped alkali-free glass fibre and flat nothing
The mixture of alkali containing glass fibre is 40 and mass ratio is 1：Material when 1 nano aluminium oxide and the mixture of nano magnesia are 0.6
The comprehensive mechanical of material is optimal, while its stretch release intensity is maximum；It can be seen that for different glass fiber and different nanometers
The selection of material and ratio collocation playing a role in the present invention.
3rd, several embodiments that can be seen that the present invention based on the result of table 6 can be met for the compound of NMT molding
Material, with very high stretch release intensity and comprehensive mechanical performance.
Each technical characteristic of embodiment described above arbitrarily can be combined, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and
Therefore can not be construed as limiting the scope of the patent.It should be pointed out that for one of ordinary skill in the art comes
Say, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (1)
1. a kind of PBT composite for NMT molding, it is characterised in that according to mass fraction meter, including following components：
100 parts of polybutylene terephthalate (PBT)；
12 parts of toughener；
40 parts of reinforcing agent；
5 parts of lubricant；
8 parts of compatilizer；
0.6 part of nano material；
0.8 part of antioxidant；And
0.8 part of coupling agent；
Wherein, the nano material is that mass ratio is 1：1 nano aluminium oxide and the mixture of nano magnesia, nano aluminium oxide
Particle diameter is 120nm, and nano magnesia particle diameter is 135nm；It is 1 that the reinforcing agent is mass ratio：3 chopped alkali-free glass fibre and
The mixture of flat alkali-free glass fibre, the alkali-free glass fibre that is chopped are a diameter of 10.5 microns, and length is 3 millimeters, flat alkali-free
Glass fiber diameter is 11.5 microns, and length is 3 millimeters；The toughener is ethylene-octene block copolymer, wherein octene
Mass content is 49%；The lubricant is watt gram silicone；The compatilizer is ethylene oxidic ester, ethylene and methyl methacrylate
Ester terpolymer；The antioxidant is BASF IRGANOX 1010；The coupling agent is glycidyl ether oxygen propyl front three
TMOS.
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| CN106995593A (en) * | 2017-04-07 | 2017-08-01 | 深圳市华盈新材料有限公司 | Nanometer injection PBT composite and its preparation technology |
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