CN109486132A - A kind of PBT direct injection molding efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules and preparation method thereof - Google Patents
A kind of PBT direct injection molding efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to modifying plastics and processing technique field more particularly to a kind of efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules and preparation method thereof that may be directly applied to the injection moulding processing of PBT product；The multifunctional mother granules are composed of two kinds of master batches of A and B, and the mass percentage composition of A master batch is as follows: 50.0~60.0wt.% of glass fibre, 30.0~40.0wt.% of Gao Liudong PBT resin, acrylic acid diglycidyl ether grafted elastomeric are from 5.0~10.0wt.% of aggressiveness, 0.1~0.3wt.% of antioxidant；Functional agglomerate prepared by the present invention is compared with conventional plastic functional agglomerate, it avoids in fire retardant PBT with no halogen resin modified system process, because modified performance mutually damages caused by mutually shearing abrasion between glass fibre and fire retardant and inorganic functional modified additive particle, it solves above-mentioned two unmatched problem of modified system processing temperature simultaneously, significantly enhances the two modified performance；The master batch has easy dispersion processing feature, and rear injection molding can be simply mixed according to the ratio with PBT resin.
Description
Technical field
The invention belongs to modifying plastics and processing technique field more particularly to one kind may be directly applied to the injection of PBT product
Efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of processing and forming and preparation method thereof.
Background technique
Implementing melt blending using double screw extruder is the conventional method for implementing modifying plastics, is squeezed using parallel dual-screw
Thermoplastic can be carried out serialization melt blending extrusion with all kinds of modified additives and made by the efficiently excellent mixing efficiency of machine out
Grain, prepared modified special material will be re-used for injecting or extrusion machine-shaping goes out various products.This technology path is not only
Effectively improve the physical mechanical properties such as intensity, toughness, rigidity, creep resistance, the warp resistance of plastic products, but also can
Assign the special physical chemistry effects such as fire-retardant plastic products, conductive, thermally conductive, magnetic conduction, antistatic, antibacterial.Although the technology road
Position of mainstream is occupied in current modifying plastics manufacture field, however in the technology implementation process, all substrates resin with change
Property additive all have to pass through twin-screw extrusion and injection moulding melt-processed thermal history twice, polymer molecular chain and its correlation
Modified additive will appear different degrees of degradation, and the Long Service Life for causing plastic products final shortens.This technology road
Line also increases process-cycle and the energy consumption of modified plastics, runs counter to the basic concept of the current sustainable industrial development of green.This
Outside, for the modified additive of different shape and different materials matter there may be the greatest differences of process unit and processing technology,
Such as high temperature high shear effect can be played using twin-screw extrusion machining, the modified performances such as activeness and quietness are performed into maximum limit
Degree；And utilize the low temperature of mixer and mediate effect for a long time, can will not heatproof auxiliary agent, low melting point auxiliary agent, low bulk density it is difficult
The various additives such as feeding powder, hygroscopic auxiliary agent, liquid and colloid auxiliary agent, whisker are sufficiently mixed and are uniformly dispersed, however adopt
It then cannot achieve such processing effect with double screw extruder melting extrusion blending.
It is in the development process of current plastics modification technology field that modified plastics is prepared by the way of plastic functional master batch
An important measures.Passed through using the functional agglomerate well prepared in advance containing high concentration modified additive and plastic raw materials double
Screw extruder or mixer implement melt blending and extruding pelletization, can not only more effectively improve point of additive in the base
It dissipates property and obtains superior modified effect, additionally it is possible to which the dust pollution for reducing processing workshop is to realize that modified plastics green adds
One of important channel of work.With the rapid development of the functionalized design and technology of preparing of plastic master batch, the function of plastic master batch
It is stronger and stronger, kind is more and more abundant, application field is also constantly expanded, and the master batch applications of modifying plastics will become not
Carry out an indispensable Key Common Technologies in modified plastics cleanly production field.
Currently, the requirement to its performance carrys out higher and higher, many application fields with the continuous expansion in plastic applications field
Plastic products are needed to have multi-functionals such as high intensity, high tenacity, high temperature resistant, fire-retardant, thermally conductive, conductive and excellent comprehensive
Can, the modified additive and auxiliary agent that add various material and form are required to the preparation processing of each modified materials, this
Great challenge is proposed to conventional plastic modification technology.Although the development of plastic functional master-batch techniques provides for this challenge
Technical support, but many technical problems are still had in the actual operation process.Wherein main technical problem includes following three
Point: 1. the modified additive and auxiliary agent of unlike material and form could need to be sent out to the maximum extent using different process units and technique
Wave its respective modified effect；2. the modified additive and auxiliary agent and matrix resin of unlike material and form are in same process unit
On (double screw extruder or mixer) implement melt blending can because its mutually shear wear caused by modified performance mutually damage；3. different
The processing temperature otherness of material modified additive and auxiliary agent and matrix resin melt blending is big, if filled simultaneously in identical processing
Standby middle implementation blending can generate serious temperature mismatch problem, and modified effect is caused to be deteriorated.Such as it is hindered for enhanced Halogen
Combustion, thermally conductive and shading multifunctional plastic System Modification, when enhancing glass fibre, nitrogen/phosphorus fire retardant, inorganic thermally conductive and shading powder
Body is simultaneously and matrix resin in double screw extruder or mixer when carrying out melt blending, understand between fiber and inorganic particulate because
Abrasion causes Fiber Aspect Ratio to decline to a great extent each other, and fiber-reinforcing effect is caused to be deteriorated；Fiber and organic fire-retardant also can be because
Internal frictional heat generation causes fire retardant to decompose, and seriously affects flame retardant effect.In addition, fiberglass reinforced plastics modified system with it is fire-retardant
There are apparent differences for the processing temperature of modified plastics system, usually enhance the processing temperature of modified system than flame-retardant system
Processing temperature is 40~70 DEG C high, if these two types of modified systems to be implemented to melting under same process unit same process conditions altogether
It is mixed, modification effect of one of system will be damaged.Modified performance mutually damages problem between above-mentioned different additive system, at present
It is especially prominent in the high performance and multifunction modification technology implementation process of plastics.
For plastics high performance and multifunction modified synchronous implementation process the problem of, invention
The thinking of double master batches is combined using function to implement the enhancing and multi-functional modified developing thought of plastics.Change for plastics
Property additive material the characteristics of, will be blended processing in there may be the additives that modified performance mutually damages to be prepared into A and two kinds of B respectively
Master batch, and the structure of the modified additive according to contained by both master batches, material and physical property feature, separately design out respective height
Dispersed system.Then two kinds of functional agglomerate synchronous applications are injection moulded in plastic products and are processed, can avoid modeling in this way
In material enhancing and functional modification process the modified additive efficiency that generates mutually damage, processing temperature mismatch problem, simultaneously
The maximum modification efficiency of unlike material modified additive and auxiliary agent is played, also can avoid traditional function master batch and matrix resin again
Extruding pelletization processing to effectively improve the effect of modifying plastics, reduce the production of production and processing period, and has saved production energy
Source consumption.This thinking will provide important approach to realize that energy-efficient green plastic is processed.
PBT is the fourth-largest engineering plastics of Present Global usage amount, by changing to PBT progress high performance and functionalization
Property, it can greatly expand its application field.As a kind of important PBT modified material, enhanced flame retardant type PBT compound is in automobile zero
The fields such as component, household, communication, electronic apparatus are widely applied.It is halogen fire-retardant with the continuous improvement of people's environmental consciousness
Application of the agent in PBT is modified is restricted, and the application of enhanced fire retardant PBT with no halogen material is promoted.Enhanced Halogen resistance
Firing thermally conductive shading modified PBT PP Pipe Compound is a kind of very important multi-functional PBT modified special material, be widely used in industry and
The manufacture of civil electric appliance shell, electronic circuit supporting element and connector and LED lamp cover and internal product.But such multi-functional
PBT modified special material, but in the processing preparation process of enhanced fire retardant PBT with no halogen modified special material, inorganic enhancing is fine
Dimension, thermal conducting agent, opacifier powder and halogen-free flame retardants are added to progress melt blending extrusion in PBT resin simultaneously, just will appear
Typical additive agent modified efficiency mutually damages phenomenon.
Summary of the invention
To solve to change present in the existing thermally conductive shading modified PBT PP Pipe Compound preparation process of glass fiber reinforced halogen-free flame-retardant
Property efficiency mutually damage problem, the present invention, which provides, a kind of may be directly applied to the efficient enhanced of PBT plastic product injection moulding processing
Halogen-free flame-retarded heat-conducting shading multifunctional mother granules and preparation method thereof.The functional agglomerate is composed of two kinds of functional agglomerates of A and B.
Wherein A master batch is mainly by glass fibre, the PBT resin of high fluidity and acrylic acid diglycidyl ether grafted elastomeric from aggressiveness group
At, by twin-screw melting extrusion be blended processing be prepared into enhancing master batch；B master batch is mainly by phosphorus-nitrogen compound flame retardant and low viscous
The ultra-dispersed property vector resin composition of aliphatic copolyester is spent, halogen-free flame-retarded heat-conducting shade function master batch is prepared as by mixer.
It can use to obtain following technical advantage with the method for processing two kinds of master batches respectively: 1. avoiding glass fibre and phosphorus/nitrogen system is fire-retardant
Agent, which is directly blended, generates internal frictional heat generation, leads to the decomposition of phosphorus/nitrogenated flame retardant；2. avoiding inorganic solid particles (thermal conducting agent
And opacifier) and glass fibre between because mutually shearing abrasion caused by Fiber Aspect Ratio decline to a great extent；3. solving glass fibers
The a variety of modified system melt blending processing temperature of dimension enhancing PBT and phosphorus-nitrogen compositional flame-retardant PBT, thermally conductive modified PBT, shading modified PBT
Spend unmatched problem；4. using acrylic acid diglycidyl ether grafted elastomeric from aggressiveness as A master batch carrier component, reaction
Property end group can have maximum touch opportunity with the end group of PBT resin in the environment of non-antiflaming powder interferes, play to greatest extent
Its toughening effect.5. not only being avoided from aggressiveness as A master batch carrier component using acrylic acid diglycidyl ether grafted elastomeric
General PE class carrier and PBT resin poor compatibility, composite material are easy the defect of peeling, moreover it is possible to it is each to improve organic-inorganic in formula
Interface adhesion between component, while it being also improved composite melt mobility, improve product surface finish and resistance
Shape ability.In addition, the physical property characteristic of the modified additive loaded for two kinds of master batches of A and B all in accordance with it, implements and promotes it
The design of the formula system of lubrication and high efficiency dispersion.Therefore, can according to performance requirement directly by A and B master batch according to a certain ratio with PBT
Rear injection molding is simply mixed in resin, can also increase the injection molding together of other resins and/or master batch: including but not limited to:
PET resin, PC resin, Masterbatch, plasticizing mother particle, nucleation master batch, chain extension master batch, lubrication master batch, antistatic master granule, anti-aging are female
Grain, conductive agglomerate, heat conduction master batch, laser carving master batch, silicone master batch, antibacterial matrices.Due to it is used in injection molding machine be that single screw rod is molten
Body promotes mode, very faint to the shear action of glass fibre, thermal conducting agent, opacifier and fire retardant, substantially will not be to the two
Modification effect damage.Therefore, this method not only effectively prevents glass fibre and thermal conducting agent, opacifier and fire retardant
Because mutually damaging again by the modified performance caused by the processing of twin-screw blending extrusion, the enhancing greatly improved to PBT is fire-retardant
Modified effect, at the same also make invention master batch to have a great design flexible, can be required to carry out according to client's difference more resins,
More master batch joint injection moldings, quickly, easily achieve the goal requirement, to practice modifying plastics formula of the 1+1 greater than 2 and processing
Process lowest optimization design concept.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of PBT direct injection molding, the functional agglomerate is by A
It is composed with two kinds of master batches of B, the mass percentage composition of the A master batch is as follows: 50.0~60.0wt.% of glass fibre, Gao Liu
Dynamic 30.0~40.0wt.% of PBT resin, acrylic acid diglycidyl ether grafted elastomeric are from 5.0~10.0wt.% of aggressiveness, antioxidant
The mass percentage composition of 0.1~0.3wt.%, the B master batch are as follows: 40.0~50.0wt.% of phosphorus flame retardant, nitrogen system are fire-retardant
15.0~30.0wt.% of agent, 10.0~20.0wt.% of thermal conducting agent, 2.0~5.0wt.% of opacifier, acrylic acid diglycidyl ether connect
Branch elastomer is from 5.0~10.0wt.% of aggressiveness, 3.0~6.0wt.% of aliphatic copolyester, 0.5~1.0wt.% of dispersing agent, lubrication
0.5~1.0wt.% of agent.
Further, the glass fibre is the fixed length chopped strand that distribution of lengths is 3.0~5.0mm.
Further, the inherent viscosity of the high flowing PBT resin is 0.76~0.85.
Further, the aliphatic copolyester is poly- (EGS ethylene glycol succinate-succinic acid-butanediol ester), poly- (fourth two
One of sour glycol ester-dimethyl succinic acid butanediol ester) and poly- (EGS ethylene glycol succinate-phenylsuccinic acid butanediol ester)
Or it is several.
Further, the acrylic acid diglycidyl ether grafted elastomeric from aggressiveness be by sodium, calcium, magnesium, barium or zinc from
The acrylic acid diglycidyl ether grafted ethene-octene-acrylic acid copolymer elasticity of son crosslinking is from aggressiveness.
Further, the antioxidant is 1,3,5- trimethyls -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene
(trade name antioxidant 1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant
It S9228 is in mass ratio) compound of 1:1 composition.
Further, the phosphorus flame retardant is diethyl hypophosphites aluminium, Methylethyl hypophosphites aluminium, polyphosphoric acids
Any one or a few in ammonium and Melamine Polyphosphate.
Further, the nitrogenated flame retardant is any one in melamine cyanurate and melamine or two
Kind.
Further, the thermal conducting agent be pulverulent boron nitride, aluminium nitride, silicon carbide, aluminum oxide, zinc oxide,
One or more of nickel oxide.
Further, the opacifier is one or more of titanium dioxide, zinc sulphide and White Carbon black.
Further, the dispersing agent is one or more of stearic acid, calcium stearate or zinc stearate.
Further, the lubricant be ethylene-vinyl acetate co-polymer wax, ethylene-acrylic copolymer wax, E wax,
One or more of OP wax, pentaerythritol stearate and dimethyl silicone polymer.
A kind of method for preparing efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of PBT direct injection molding,
The method is related to the preparation method of A master batch and B master batch, the preparation method of the A master batch the following steps are included:
(1) weigh according to the ratio glass fibre, Gao Liudong PBT resin, acrylic acid diglycidyl ether grafted elastomeric from aggressiveness and
Antioxidant, and height flowing PBT resin, aliphatic copolyester, acrylic acid diglycidyl ether grafted elastomeric from aggressiveness and are resisted
Oxygen agent puts into super mixer and is uniformly mixed；
(2) mixture obtained in step (1) is measured into feeding double screw extruder from main feeder, short glass fiber is led to
Side feeder metering feeding double screw extruder is crossed, blending extrusion is carried out and is granulated, obtain the A master batch.
Further, the barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is
250~300 revs/min.
Further, the barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is
150~200 revs/min；The mould-cavity temperature control of impregnation mold at 275~285 DEG C, dragger speed control 50~70 meters/
Minute.
A kind of method for preparing efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of PBT direct injection molding,
The method is related to the preparation method of A master batch and B master batch, the preparation method of the B master batch the following steps are included:
(1) phosphorus flame retardant, nitrogenated flame retardant, thermal conducting agent, opacifier, aliphatic copolyester, acrylic acid two is weighed according to the ratio to contract
Water glycerin ether grafted elastomeric is put into super mixer and is shifted after mixing from aggressiveness, dispersing agent and lubricant
Hot milling is carried out in mixer, obtains bulk blend；
(2) the bulk blend obtained in step (1) is fed into single screw extrusion machine by taper feeder, is squeezed out simultaneously through melting
It is granulated, obtains the B master batch.
Further, the melting temperature of mixer is 120~135 DEG C, and mixing time is 15~20 minutes；Single screw rod squeezes out
The screw speed of machine is 150~200 revs/min, and barrel temperature is 155~165 DEG C.
It is using the beneficial effect of technical solution of the present invention:
It (1) is by the way of A master batch and the preparation of B master batch separate machined, to prepare respectively for the physical property feature of modified additive
Glass fiber reinforcement master batch (A master batch) and the thermally conductive shading master batch of phosphorus-nitrogen compositional flame-retardant (B master batch), effectively prevent PBT and glass
When glass fiber and thermally conductive, shading and the direct melt blending of a variety of modified additives of halogen-free flameproof squeeze out, because of mutual shearing, wear and
It is impaired with enhancing caused by halogen-free flame retardants decomposition and flame-retarded efficiency that frictional heat generation causes glass fibre draw ratio to reduce, while
Solve two unmatched technical problems of modified system processing temperature, so that it is respective to significantly improve two kinds of modified additives
Modified performance.
(2) it is all made of in A and B master batch with polymolecularity and high-compatibility resin joint vector, not only effectively improves
The interface adhesion and its dispersibility in resin matrix of glass fibre, thermal conducting agent and opacifier and PBT resin, moreover it is possible to benefit
With the high flow behavior of these carriers, prepared A and B master batch is directly used in the injection moulding processing of PBT plastic product, and obtains
Superior enhancing, fire-retardant, thermally conductive and shaded effect.
(3) multifunctional mother granules prepared by the present invention are ingenious to have used two kinds of differences compared with conventional plastic functional agglomerate
The combination of functional agglomerate is processed respectively, and it is modified to not only solve different additive in modified plastics preparation process
The problem that efficiency is mutually damaged, produces the modified effect that 1+1 is much larger than 2, also has easily dispersion easy processing feature, can be moulded according to PBT
The performance requirement of material products directly applies to plastics system after A master batch and B master batch are simply mixed with PBT resin according to a certain ratio
The injection moulding of product is processed.Due to it is used in injection molding machine be that single screw rod melt promotes mode, to glass fibre and fire retardant
Shear action is very faint, substantially will not modification effect to the two damage, so as to avoid common plastics modifying process
In matrix resin and modified master batch be secondary or the multiple melting mixing by processing equipment caused by antioxidant loss, enhancing
Fiber Aspect Ratio loss and matrix resin thermal cracking problem, significantly improve the mechanical performance and long-time service of PBT product.
(4) present invention is effectively improving the PBT enhancing multiple modified efficiency of halogen-free flame-retarded heat-conducting shading simultaneously, simplifies plastics
Modified procedure of processing reduces the process-cycle, reduces energy consumption, improves production efficiency, is truly realized green chemical industry development
Theory.Combination type functional master batch of the invention can flexibly be adjusted according to customer requirement in PBT plastic product process of injection molding
Combination with A master batch and B master batch and its its performance and cost are adjusted with the proportion of resin raw material.Method of the invention and
Technology can be widely applied to all kinds of PBT plastic products injection moulding and high performance and functional modification integration processing.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but these embodiments are not
Limiting the scope of the invention." one embodiment " or " embodiment " referred to herein, which refers to, may be included in the present invention at least
A particular feature, structure, or characteristic in one implementation.In the present specification different places occur " in one embodiment
In " the same embodiment not is referred both to, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 250 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 130 DEG C, and mixing time is 20 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 185 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
Embodiment 2
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 300 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 130 DEG C, and mixing time is 18 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 165 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
Embodiment 3
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 280 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 120 DEG C, and mixing time is 20 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 170 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
Embodiment 4
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 280 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 125 DEG C, and mixing time is 18 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 150 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
Embodiment 5
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 280 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 120 DEG C, and mixing time is 18 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 200 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
Embodiment 6
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of a kind of PBT resin direct injection molding, by A and two kinds of B
Master batch is composed, and the raw material mass mixture ratio of A master batch is as follows:
Antioxidant is 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (trade name antioxidant
1330) and bis- (2,4-dicumylphenyl) pentaerythritol diphosphites (trade name antioxidant S9228) are 1 in mass ratio:
The compound of 1 composition.
The raw material mass mixture ratio of its B master batch is as follows:
A master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, then will be in addition to glass fibre
It is uniformly mixed in all raw material investment high-speed mixers, then obtained mixture is measured into feeding twin-screw extrusion from main feeder
Machine carries out blending extrusion and is granulated, described in acquisition by short glass fiber by side feeder metering feeding double screw extruder
A master batch；The barrel of double screw extruder to head temperature of each section is controlled at 230~275 DEG C, and screw speed is 280 revs/min.
B master batch the preparation method is as follows: weigh all raw materials by above-mentioned quality proportioning requirement, and put into mixed at high speed
It is transferred to after mixing in device in mixer and carries out hot milling, the melting temperature of mixer is 135 DEG C, and mixing time is 15 points
Clock feeds single screw extrusion machine by taper feeder, squeezes out and be granulated through melting, obtain then by acquired bulk blend
Obtain the B master batch；The screw speed of single screw extrusion machine is 175 revs/min, and barrel temperature Discrete control is at 155~165 DEG C.
A master batch and B master batch are mixed according to any mass ratio in the present invention, unknown between the component in remaining place in the present invention
The expression for really writing proportionate relationship exactly is able to achieve according to arbitrary proportion.
To verify the efficient enhanced more function of halogen-free flame-retarded heat-conducting shading of PBT resin direct injection molding prepared by the present invention
A master batch prepared by embodiment 1-6 and B master batch, are pressed the quality hundred of 25wt.% and 35wt.% by the modified effect of energy master batch respectively
Ratio is divided to mix simultaneously with PBT resin, direct injection forms test bars, then carries out properties detection；At the same time, according to
The identical component of injection test bars and proportion are obtained in embodiment 1-6, and are infused again after processing is blended by double screw extruder
Type test bars are moulded into as reference examples, then its performance is detected.All properties test result is as shown in table 1 (wherein
Reference examples 1-6 is molded into again after respectively and in embodiment 1-6 forming but use twin-screw extrusion machining identical as proportion
The performance of type test bars).
By the reference to data in table 1 show by PBT resin direct injection prepared by above embodiments of the present invention at
The efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of type, after being applied to the molding of PBT resin direct injection, in component
And in the identical situation of proportion, tensile strength, notch impact strength and the flame retardant property of plastic products, hence it is evident that better than use
The performance of injection moulded products again after twin-screw extrusion machining.Using functional agglomerate of the invention, not only will greatly simplify
The modified procedure of processing of PBT resin improves processing efficiency, reduces energy consumption, also significantly enhances modified effect, realizes modeling
The sustainable development theory of material preparation green processing.
Functional agglomerate direct injection prepared by 1 embodiment 1-6 of table forms PBT resin test bars and same materials formula
It is injection moulded the performance control of PBT resin test bars again through twin-screw extrusion machining
Table 1
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff completely may be used
Without departing from the scope of the technological thought of the present invention', to carry out various changes and amendments.It is all in spirit of the invention and
Within principle, any modification, equivalent substitution, improvement and etc. done be should all be included in the protection scope of the present invention.This item hair
Bright technical scope is not limited to the contents of the specification, it is necessary to its technical model is determined according to scope of the claims
It encloses.
Claims (10)
1. a kind of efficient enhanced halogen-free flame-retarded heat-conducting shading multifunctional mother granules of PBT direct injection molding, it is characterised in that: institute
It states multifunctional mother granules to be composed of two kinds of master batches of A and B, the mass percentage composition of the A master batch is as follows: glass fibre 50.0
30.0~40.0wt.% of~60.0wt.%, Gao Liudong PBT resin, acrylic acid diglycidyl ether grafted elastomeric from aggressiveness 5.0~
10.0wt.%, 0.1~0.3wt.% of antioxidant, the glass fibre are the fixed length chopped strand that distribution of lengths is 3.0~5.0mm,
The inherent viscosity of the high flowing PBT resin is 0.76~0.85,
The mass percentage composition of the B master batch is as follows: 40.0~50.0wt.% of phosphorus flame retardant, nitrogenated flame retardant 15.0~
30.0wt.%, 10.0~20.0wt.% of thermal conducting agent, 2.0~5.0wt.% of opacifier, acrylic acid diglycidyl ether grafted elastomeric
From 5.0~10.0wt.% of aggressiveness, 3.0~6.0wt.% of aliphatic copolyester, 0.5~1.0wt.% of dispersing agent, lubricant 0.5~
1.0wt.%。
2. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 1
Master batch, it is characterised in that: the aliphatic copolyester is poly- (EGS ethylene glycol succinate-succinic acid-butanediol ester), poly- (succinic acid
Glycol ester-dimethyl succinic acid butanediol ester) and one of poly- (EGS ethylene glycol succinate-phenylsuccinic acid butanediol ester) or
It is several.
3. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 1
Master batch, it is characterised in that: the acrylic acid diglycidyl ether grafted elastomeric is by sodium, calcium, magnesium, barium or zinc ion from aggressiveness
The acrylic acid diglycidyl ether grafted ethene-octene-acrylic acid copolymer elasticity of crosslinking is from aggressiveness.
4. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 1
Master batch, it is characterised in that: the antioxidant is 1,3,5- trimethyls -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene
It is in mass ratio the compound of 1:1 composition with bis- (2,4-dicumylphenyl) pentaerythritol diphosphites.
5. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 1
Master batch, it is characterised in that: the phosphorus flame retardant is diethyl hypophosphites aluminium, Methylethyl hypophosphites aluminium, polyphosphoric acids
Any one or a few in ammonium and Melamine Polyphosphate；The nitrogenated flame retardant is melamine cyanurate and three
Any one in poly cyanamid or two kinds, the inorganic fire-retarded synergist be in antimony oxide and zinc borate any one or
Two kinds, the thermal conducting agent is one of the boron nitride of powder shaped, aluminium nitride, silicon carbide, aluminum oxide, nickel oxide or several
Kind, the opacifier is one or more of titanium dioxide, zinc oxide, zinc sulphide and White Carbon black.
6. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 1
Master batch, it is characterised in that: the dispersing agent is one or more of stearic acid, calcium stearate or zinc stearate；The lubrication
Agent is ethylene-vinyl acetate co-polymer wax, ethylene-acrylic copolymer wax, E wax, OP wax, pentaerythritol stearate and gathers
One or more of dimethyl silica.
7. a kind of preparation PBT direct injection molding as described in any one of claim 1-6 is led with efficiently enhanced halogen-free flameproof
The method of hot shading multifunctional mother granules, it is characterised in that: the preparation method of the A master batch the following steps are included:
(1) glass fibre, Gao Liudong PBT resin, aliphatic copolyester, acrylic acid diglycidyl ether grafting bullet are weighed according to the ratio
Property body from aggressiveness and antioxidant, and by height flow PBT resin, aliphatic copolyester, acrylic acid diglycidyl ether grafted elastomeric
Body is uniformly mixed from aggressiveness and antioxidant investment super mixer；
(2) mixture obtained in step (1) is measured into feeding double screw extruder from main feeder, short glass fiber is led to
Side feeder metering feeding double screw extruder is crossed, blending extrusion is carried out and is granulated, obtain the A master batch.
8. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 7
The preparation method of master batch, it is characterised in that: the processing technology of the A master batch are as follows: the barrel of double screw extruder is to each section of head
At 230~275 DEG C, screw speed is 250~300 revs/min for temperature control.
9. a kind of preparation PBT direct injection molding as described in any one of claim 1-6 is led with efficiently enhanced halogen-free flameproof
The method of hot shading multifunctional mother granules, it is characterised in that: the preparation method of the B master batch the following steps are included:
(1) phosphorus flame retardant, nitrogenated flame retardant, thermal conducting agent, opacifier, aliphatic copolyester, acrylic acid two is weighed according to the ratio to contract
Water glycerin ether grafted elastomeric is put into super mixer and is shifted after mixing from aggressiveness, dispersing agent and lubricant
Hot milling is carried out in mixer, obtains bulk blend；
(2) the bulk blend obtained in step (1) is fed into single screw extrusion machine by taper feeder, is squeezed out simultaneously through melting
It is granulated, obtains the B master batch.
10. a kind of PBT direct injection molding is multi-functional with efficient enhanced halogen-free flame-retarded heat-conducting shading according to claim 9
The preparation method of master batch, it is characterised in that: the processing technology of the B master batch are as follows: the melting temperature of mixer is 120~135 DEG C,
Mixing time is 15~20 minutes；The screw speed of single screw extrusion machine be 150~200 revs/min, barrel temperature be 155~
165℃。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480610A (en) * | 2020-11-26 | 2021-03-12 | 上海金发科技发展有限公司 | High-impact-length basalt fiber reinforced halogen-free flame-retardant PBT material and preparation method thereof |
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| CN103160080A (en) * | 2011-12-14 | 2013-06-19 | 合肥杰事杰新材料股份有限公司 | A halogen free flame retardant long glass fiber reinforced PBT composite material and a preparation method thereof |
| CN106633681A (en) * | 2015-08-04 | 2017-05-10 | 东丽先端材料研究开发（中国）有限公司 | High-toughness polyester resin alloy composition and preparation method thereof |
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| EP0180472A2 (en) * | 1984-10-31 | 1986-05-07 | Celanese Corporation | Novel thermoplastic polyester compositions having improved impact behaviour |
| CN1810862A (en) * | 2006-02-23 | 2006-08-02 | 广州金发科技股份有限公司 | Continuous long fiber reinforced fire-retardant thermoplastic resin and its prepn |
| CN103160080A (en) * | 2011-12-14 | 2013-06-19 | 合肥杰事杰新材料股份有限公司 | A halogen free flame retardant long glass fiber reinforced PBT composite material and a preparation method thereof |
| CN106633681A (en) * | 2015-08-04 | 2017-05-10 | 东丽先端材料研究开发（中国）有限公司 | High-toughness polyester resin alloy composition and preparation method thereof |
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| CN112480610A (en) * | 2020-11-26 | 2021-03-12 | 上海金发科技发展有限公司 | High-impact-length basalt fiber reinforced halogen-free flame-retardant PBT material and preparation method thereof |
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