CN105273368B - A kind of expandable PET resin and its production and use - Google Patents
A kind of expandable PET resin and its production and use Download PDFInfo
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Abstract
The present invention discloses a kind of expandable PET resin and its production and use.The preparation method includes：(1) raw material components are well mixed, it includes 985~995 parts of physiochemical mutagens PET bottle piece, 1~9 part of chain extender, 1~3 part of antioxidant, 1~3 part of heat stabilizer；Described chain extender is by polyfunctional group chain extension monomer in mass ratio 1 that trifunctional chain extension monomer and functional group number are 4~6:3~5:1 compounding；(2) melting extrusion is granulated；(3) by resulting material under 210~230 DEG C, 5~100Pa vacuums 1~5h of solid phase polycondensation, obtain expandable PET resin.Expandable PET resin molecular weight of the invention is big, molecular weight distribution is wide, melt strength is high, change the use such as physiochemical mutagens PET drop, and low raw-material cost, preparation process is simple, it is combined by chain extender, using reactive extrursion combination solid phase polycondensation, reaction time, more conducively industrialized production are shortened.
Description
Technical field
The present invention relates to a kind of polyester foam materials, more particularly to a kind of expandable PET resin and preparation method thereof and
Purposes.
Background technology
Polyethylene terephthalate (PET) is yield maximum, the cheapest kind of price in thermoplastic polyester, is had
Excellent physics, chemistry and mechanics mechanical performance, three big field of synthetic fibers, biaxially oriented film and polyester bottles is widely used in,
Wide application prospect is also show in foamed material field in recent years.PET polyester foam materials have light weight, specific strength
Greatly, rigidity is big, electrical insulating property is good and the advantages that sound deadener/insulator, can be applied to packaging for foodstuff, construction material, wire insulation, micro-
The fields such as ripple container, refrigerator inner panel, sports equipment, automobile, space flight.China PET polyester total output is about 1~3,000 ten thousand at present
Ton/year.Because PET polyester products are mostly disposable products or easily-consumed products, with substantial amounts of discarded object during production and use,
And PET discarded objects are unable to spontaneous degradation, serious environmental pollution and the wasting of resources are easily caused.Therefore the recovery of PET discarded objects
Had important practical significance with regeneration.
PET Polyester waste recovery methods mainly have chemical recovery and physiochemical mutagens.Chemical recovery is by sugar solution, alcoholysis
With the method for hydrolysis, PET polyester is decomposed into oligomer and monomer, then regrouped as PET polyester.Although it can realize that PET gathers
The complete cycling and reutilization of ester discarded object, but cost is larger, can not large-scale promotion.Physiochemical mutagens method is to gather waste PET
Ester through classification, crush, wash and drying process after carry out reconstruction grain, there is provided give fiber factory as production fiber raw material.
But increasing with processing times, inherent viscosity, molecular weight distribution and the impurity content of PET polyester all can constantly change, lead
Cause physiochemical mutagens limited using number.Therefore simple physiochemical mutagens method is actually a kind of by the unidirectionally recovery such as drop of PET polyester
Application way, i.e. bottle piece-fiber, fiber-dead meal, there is no method to realize that complete closed loop recycles.
Conventional PET polyester due to industry melting it is continuous foamed during, melt strength, melt viscosity and tensile viscosity compared with
Small, melt rheological property can be poor, can not support the growth and sizing of abscess；And PET polyester at high temperature easily occur hydrolysis,
Pyrolysis and thermal oxidative degradation, cause to cannot get good abscess in foaming process.And PET polyester is because of spy made from physiochemical mutagens method
Property viscosity is low, impurity content is high, further increases the technical difficulty for preparing foaming PET resin.Therefore, to overcome physiochemical mutagens
The defects of PET polyester, Pillar recovery must be modified, improve the molecular weight of PET polyester, widen molecular weight distribution, increase length
Chain branching degree, to obtain the foaming PET resin with good foam structure by melt foaming.
Existing PET polyester recovery is modified mainly to use chemical thickening method, is typically realized with the process of reactive extrursion.
Chain extending reaction is generally carried out using chemical chain extender and recycled PET exposed terminated groupses in the molten state, increases PET molecular weight, from
And improve PET inherent viscosity.Geroge P are prepared for 2,2 '-(Isosorbide-5-Nitrae-phenylene) double (bisoxazolines), and make chain extension with it
Agent, recycled PET beverage bottle is modified.After Pillar recovery PET viscosity is increased to thickening by the 0.69dL/g before viscosifying
0.85dL/g, good Efficient Adhesive Promotion [Journal of applied polymer science, 2000,77 (6) are reached:
2206-2211].Domestic relevant report is also a lot, 2,2- double (2- bisoxazolines) (BOZ) and the phthalic anhydrides such as Cai Changgeng
(PA) combination is modified to the Pillar recovery PET that inherent viscosity is 0.411dL/g, when alone BOZ chain extensions Pillar recovery PET's
Inherent viscosity increases about 10%, reaches 0.457dL/g, and inherent viscosity has reached 0.695dL/g after BOZ and PA combinations, carries
It is high by nearly 75%.Therefore, the purpose that thickening is modified to Pillar recovery PET is preferably realized using method associated with chain extender
[plastics, 2005,34 (2):63-66].By reactive extrursion, PET inherent viscosity increased, and can reach industrial processes
It is required that.But because reactive extrursion can not bring up to PET melt strength the intensity needed for foaming, so modified
PET is not suitable for still foaming, and does not reach the requirement of foaming.The reinforcing agent such as He Jianxin, toughener, fire retardant, clay, nucleation
Agent, antioxidant proportioning, are extruded by double screw extruder, the high PET of obtained high performance, high intensity, energy-conserving and environment-protective, anti-flammability
Expect [Chinese invention patent, CN201010196709.5].And it is modified by toughener etc., although the physical strength of energy REINFORCED PET,
But molecular structure is not appropriate for foaming.Therefore, such as a kind of how inexpensive, capable of being industrialized mode, recycled PET polyester is utilized
For raw material, expandable PET resin is prepared, is the technical problem that need to be solved by the researchers in the field.
The content of the invention
The technical problems to be solved by the invention are to overcome that existing physiochemical mutagens PET molecular weight of polyesters is low, and melt is strong
Degree is poor, and normal foaming is difficult in reactive extrursion and simple toughener chemical modification PET molecular structures are not suitable for foaming
A kind of defect, there is provided expandable PET resin and its production and use.The expandable PET resin of the present invention is returned with physics
It is raw material to receive PET bottle piece, and cost is cheap, and preparation process is simple, is combined by chain extender, using reactive extrursion and solid phase polycondensation two
Individual process, PET melt strength is effectively increased, shorten the reaction time of conventional solid polycondensation, more conducively industrialized production.
And the expandable PET resin molecular weight for preparing of the present invention is big, molecular weight distribution is wide, melt strength is high, not only changes physics
Drop of recycled PET etc. uses, and the introduction of solid phase polycondensation process, reduces the presence of small molecule, reduces side reaction so that
Modified PET has good foam performance, available for preparation PET foamed products.
The invention provides a kind of preparation method of expandable PET resin, it comprises the following steps：
(1) raw material components are mixed evenly；Described raw material components include physiochemical mutagens PET bottle piece 985~995
Part, 1~9 part of chain extender, 1~3 part of antioxidant, 1~3 part of heat stabilizer；Described chain extender by trifunctional chain extension monomer with
Polyfunctional group chain extension monomer in mass ratio 1:3~5:1 is compounded, and described polyfunctional group chain extension monomer is functional group number 4
~6 chain extension monomer；
(2) the material melts extruding pelletization for being well mixed step (1)；
(3) step (2) is granulated obtained material 1~5h of solid phase polycondensation under 210~230 DEG C, 5~100Pa vacuums,
Obtain expandable PET resin.
In step (1), described physiochemical mutagens PET bottle piece is the PET bottle piece that this area Typical physical absorption method obtains；Institute
The fusing point for the physiochemical mutagens PET bottle piece stated is preferably 252~256 DEG C, and initial intrinsic viscosity is preferably 0.6~0.7dL/g.
In step (1), described physiochemical mutagens PET bottle piece is preferably by drying pretreatment；Described dries pretreatment
Preferably use following step：First 100~120 DEG C of dry 10~15h in convection oven, are then transferred in vacuum drying oven,
120~150 DEG C of 10~15h of vacuum drying.
In step (1), described chain extender is the conventional chain extender in this area；Described trifunctional chain extender is preferably
For triglycidyl isocyanurate (TGIC), described polyfunctional group chain extension monomer is preferably the equal benzene of four-functional group chain extender
Tetracarboxylic acid anhydride (PMDA) and/or six functional groups chain extender ADR4370.
In step (1), described antioxidant is the conventional antioxidant in this area, preferably antioxidant 1010 and/or anti-
Oxygen agent 168；The fusing point of described antioxidant 1010 is 110.0~125.0 DEG C, density 1.15g/cm3, described antioxidant
168 fusing point is 182~186 DEG C, density 1.03g/cm3。
In step (1), described heat stabilizer is the conventional heat stabilizer in this area, preferably triphenyl phosphite
And/or triethylene thiophosphoramide (TEPA) (TPP)；Described heat stabilizer TPP fusing point is 22~24 DEG C, relative molecular weight
For 310.29, density 1.184g/cm3, described heat stabilizer TEPA fusing point is -40 DEG C, density 0.998g/cm3。
In step (2), it is this area routine operation that described melting extrusion, which is granulated, is preferably entered using double screw extruder
OK；One area's temperature of described double screw extruder be preferably 255~275 DEG C, two area's temperature be preferably 255~275 DEG C,
Three area's temperature be preferably 260~280 DEG C, four area's temperature be preferably 260~280 DEG C, five area's temperature be preferably 255~
275 DEG C, six area's temperature be preferably 255~275 DEG C；Described double screw extruder feeding machine feeding frequency is preferably 10~
20Hz, main frame rotational frequency are preferably 10~20Hz.
In step (3), before described solid phase polycondensation is carried out, described material preferably passes through drying process；Described
Drying process preferably uses following step：First 100~120 DEG C of dry 10~15h in convection oven, are then transferred to vacuum
In baking oven, 100~120 DEG C of 10~15h of vacuum drying.
Present invention also offers one kind expandable PET resin as made from the above method.
The expandable PET resin of the present invention has long chain branched, and molecular weight is big, molecular weight distribution is wide, melt strength
It is high.Expandable PET resin inherent viscosity >=0.8dL/g of the present invention, melt index≤25g/10min.
Present invention also offers a kind of purposes of PET resin expandable as made from the above method in PET foamed products.
According to common sense in the field, expandable PET resin of the invention is foamed using the conventional operating method in this area,
For example with melting batch-foamed method and/or micropore injection moulding shaping foam method.
It on the basis of common sense in the field is met, above-mentioned each optimum condition, can be combined, it is each preferably real to produce the present invention
Example.
Agents useful for same and raw material of the present invention are commercially available.
The positive effect of the present invention is：
1st, the present invention is modified with combination chain extender, antioxidant, heat stabilizer blending extrusion by physiochemical mutagens PET bottle piece and tied
Process for solid state polycondensation is closed, the use such as physiochemical mutagens PET drop is changed, the good foam performances of PET is imparted, available for preparing
PET foamed products.
2nd, for the present invention using physiochemical mutagens PET bottle piece as raw material, being prepared by twin-screw reactive extrursion and process for solid state polycondensation can
Foaming PET resin, cost is cheap, low for equipment requirements, and preparation process is simple, is advantageous to industrialized production.
3rd, expandable PET resin prepared by the present invention, the relatively simple modified method of extrusion, melt strength are higher；More simple solid phase
Condensation methods, the polycondensation time is shorter, has reduced the number of the operation cycle significantly.
Brief description of the drawings
Fig. 1 is the complex viscosity figure of PET resin prepared by embodiment 1~2 and comparative example；
Fig. 2 is the springform spirogram of PET resin prepared by embodiment 1~2 and comparative example；
Fig. 3 is the viscous modulus figure of PET resin prepared by embodiment 1~2 and comparative example；
Fig. 4 is the expandable PET resin (c, d) of the preparation of embodiment 2 and the PET bottle piece base-material (a, b) of comparative example in difference
SEM photograph after being foamed under blowing temperature：(a) 265 DEG C, 275 DEG C of (b), 265 DEG C of (c), 275 DEG C of (d)；
Fig. 5 is SEM photograph of the expandable PET resin of the preparation of embodiment 1 under 265 DEG C of blowing temperatures.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to described reality
Apply among a scope.The experimental method of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product specification selects.
In following embodiments：
Described pyromellitic dianhydride (PMDA) is provided by Shanghai Ao highland barleys Industrial Co., Ltd., commercially available；Six described functions
Group's chain extender (ADR4370) is completed bio tech ltd by citizen of Guangzhou City and provided, commercially available.Described isocyanuric acid three shrinks sweet
Grease (TGIC), antioxidant 1010, irgasfos 168, triphenyl phosphite (TPP) and triethylene thiophosphoramide (TEPA) by
Chemical Reagent Co., Ltd., Sinopharm Group provides, commercially available.
In following embodiments, the fusing point of physiochemical mutagens PET bottle piece is 252~256 DEG C, initial intrinsic viscosity is 0.6~
0.7dL/g。
Embodiment 1
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 100 DEG C of dry 13h, transfer to 135 DEG C of vacuum in vacuum drying oven
14h is dried, obtains physiochemical mutagens PET bottle piece；
2nd, 4kg physiochemical mutagens PET bottle pieces are weighed, 12g TGIC, 4g PMDA, 4g antioxidant 1010s, 4g TPP, mixing is
Input double screw extruder extruding pelletization after even；Control each section of temperature of double screw extruder exists：One 260 DEG C of area, 260 DEG C of 2nd area,
Three 265 DEG C of areas, 265 DEG C of 4th area, 260 DEG C of 5th area, 260 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, main frame turn
Dynamic frequency 13.5hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 120 DEG C of dry 12h, take out and carry out solid phase polycondensation,
Wherein 220 DEG C of reaction temperature, vacuum 20Pa, polycondensation time 2h.
Embodiment 2
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece；
2nd, 2kg physiochemical mutagens PET bottle pieces are weighed, 8g TGIC, 2g PMDA, 2g antioxidant 1010s, 2g TPP, are well mixed
Double screw extruder extruding pelletization is put into afterwards；Control each section of temperature of double screw extruder exists：One 255 DEG C of area, 255 DEG C of 2nd area, three
255 DEG C of area, 265 DEG C of 4th area, 265 DEG C of 5th area, 265 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, main frame rotate
Frequency 13.5hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 100 DEG C of dry 15h, take out and carry out solid phase polycondensation,
Wherein 220 DEG C of reaction temperature, vacuum 10Pa, polycondensation time 4h.
Embodiment 3
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece；
2nd, 2kg physiochemical mutagens PET bottle pieces, 6g TGIC, 1g ADR4730,2g irgasfos 168s, 3g TEPA, mixing are weighed
Input double screw extruder extruding pelletization after uniformly；Control each section of temperature of double screw extruder exists：One 260 DEG C of area, two areas 265
DEG C, 270 DEG C of 3rd area, 265 DEG C of 4th area, 260 DEG C of 5th area, 260 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, master
Machine rotational frequency 13.5hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 110 DEG C of dry 12h, take out and carry out solid phase polycondensation,
Wherein 210 DEG C of reaction temperature, vacuum 20Pa, polycondensation time 1h.
Embodiment 4
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece；
2nd, 2kg physiochemical mutagens PET bottle pieces, 5g ADR4370,2g TGIC, 6g antioxidant 1010s, 3g TEPA, mixing are weighed
Input double screw extruder extruding pelletization after uniformly；Control each section of temperature of double screw extruder exists：One 265 DEG C of area, two areas 260
DEG C, 265 DEG C of 3rd area, 270 DEG C of 4th area, 265 DEG C of 5th area, 260 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, master
Machine rotational frequency 13.5hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 110 DEG C of dry 12h, take out and carry out solid phase polycondensation,
Wherein 230 DEG C of reaction temperature, vacuum 20pa, polycondensation time 5h.
Embodiment 5
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece；
2nd, 1kg physiochemical mutagens PET bottle pieces, 5g ADR4370,4g TGIC, 1g antioxidant 1010s, 2g TEPA, mixing are weighed
Input double screw extruder extruding pelletization after uniformly；Control each section of temperature of double screw extruder exists：One 265 DEG C of area, two areas 260
DEG C, 265 DEG C of 3rd area, 270 DEG C of 4th area, 265 DEG C of 5th area, 260 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, master
Machine rotational frequency 13.5hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 110 DEG C of dry 12h, take out and carry out solid phase polycondensation,
Wherein 220 DEG C of reaction temperature, vacuum 20pa, polycondensation time 3h.
Embodiment 6
A kind of preparation method of expandable PET resin, it comprises the following steps：
1st, by discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece；
2nd, 2kg physiochemical mutagens PET bottle pieces are weighed, 1g PMDA, 1g TGIC, 3g irgasfos 168s, 6g TPP, are well mixed
Double screw extruder extruding pelletization is put into afterwards；Control each section of temperature of double screw extruder exists：One 265 DEG C of area, 265 DEG C of 2nd area, three
270 DEG C of area, 270 DEG C of 4th area, 270 DEG C of 5th area, 265 DEG C of 6th area；Double screw extruder feeding machine rotational frequency 15hz, main frame rotate
Frequency 15hz；
3rd, grain will be extruded respectively in convection oven and vacuum drying oven after 110 DEG C of dry 12h, take out and carry out solid phase polycondensation,
Wherein 210 DEG C of reaction temperature, vacuum 20pa, polycondensation time 4h.
Comparative example
A kind of preparation method of PET resin, it comprises the following steps：
By discarded PET bottle piece in convection oven 110 DEG C of dry 12h, transfer to 140 DEG C of dryings in vacuum drying oven
12h, obtain physiochemical mutagens PET bottle piece base-material.
Effect example 1
The PET bottle piece base-material of expandable PET resin and comparative example prepared by embodiment 1~6 is contrasted, and is tested respectively
Inherent viscosity and melt index.Described inherent viscosity is tested using Ubbelohde viscometer, using mass ratio as (50:50) benzene
Phenol, the mixed liquor of tetrachloroethanes are solvent, and the solution for being made into 0.5% (wt.%) is with capillary diameter at 25 ± 0.1 DEG C
0.7~0.8mm determination of ubbelohde viscometer.Described melt index uses Shanghai Si Erda scientific instrument Co., Ltd RL-
11B1 types Melt Flow Rate Measurer is tested using ASTM1238 standards, and melting means instrument temperature first is set as into 260 DEG C before test,
Stroke selection 3.175, after temperature stabilization, is put into 3~5g material, is rapidly compacted material with compressing rod, excludes air
Influence, after material melts 5min, start to test, binder counterweight selection 2160g (T-shaped counterweight+material bar assembly).Test result is shown in
Table 1.
Influence of the different process of table 1 to PET inherent viscosities and melt index
As can be seen from Table 1, PET resin produced by the present invention, inherent viscosity is respectively increased to 0.95 from 0.70dL/g,
1.15th, 0.88,0.93,0.91 and 0.89dL/g, melt index are reduced to 9.8,3.7,13.5,11.3,12.1 and from 34
13.4g/10min.Modified physiochemical mutagens PET inherent viscosity is obviously improved, melt strength increase.The wherein material of embodiment 2
Numerically all meet foaming necessary requirement in inherent viscosity and melt index, there is very high melt strength.
Effect example 2
The PET bottle piece base-material of expandable PET resin and comparative example prepared by Examples 1 and 2 is contrasted, and is determined respectively
Rheological property.Described rheological property is tested using the plate rheometers of HAKKE MAR III, 275 DEG C of temperature, test frequency
0.1~100rad/s.Test result is shown in Fig. 1~3, and the stream of material is evaluated by complex viscosity, modulus of elasticity and viscous modulus
Become performance.
PET resin complex viscosity, modulus of elasticity, viscous modulus are all higher than made from embodiment it can be seen from Fig. 1~3 2
PET resin made from embodiment 1, and the PET resin complex viscosity of embodiment 2 has exceeded 10000 order of magnitude in low frequency range,
Shear shinning clearly, illustrates that modified effect is notable.
Effect example 3
The PET bottle piece base-material of expandable PET resin and comparative example prepared by embodiment 1~2 is contrasted, and passes through melting
Batch process and/or the micropore injection moulding method of forming evaluate foaming effect.Described melt foaming process 265 DEG C of blowing temperature~
275 DEG C, blow pressure 16MPa, saturation time 30min, carry out under quick pressure releasing.Described micropore injection moulding shaping foam process exists
MuCell operating platforms, melten gel 30~36mm of amount, injection speed 60%~90%, foaming agent supercritical nitrogen content 0.2%~
0.8%, 265~280 DEG C of melt temperature, carry out at 30~90 DEG C of mold temperature.Described foaming effect uses JEOL's strain
Formula commercial firm JSM-6360LV type scanning electron microscopic observation cell morphologies are analyzed, test before first by sample in liquid nitrogen cold quenching, then
Metal spraying is to strengthen its electric conductivity on sample section.The average pore size of foamed sample is divided SEM photograph by winroof softwares
Analyse and obtain.
Fig. 4 is the SEM photograph of the melting batch process foaming of comparative example and embodiment 2, wherein (a, b) is the PET of comparative example
SEM photograph of the bottle piece base-material under 265 DEG C and 275 DEG C of blowing temperatures, (c, d) are the PET resin of the preparation of embodiment 2 at 265 DEG C
With the SEM photograph under 275 DEG C of blowing temperatures.As can be seen that unmodified physiochemical mutagens PET bottle piece is because melt strength is low, nothing
The growth of method support abscess wherein, thus can not foaming.And PET resin made from embodiment 2 has good foaming
Performance, and abscess-size is more uniform.PET resin made from this explanation embodiment 2 has higher melt strength.
Fig. 5 is that the SEM of micropore injection moulding method of forming foaming of the expandable PET resin of the preparation of embodiment 1 at 265 DEG C shines
Piece.It can be seen that PET foaming products have more uniform foam structure made from embodiment 1, but cell density is smaller, hair
It is relatively low to steep multiplying power.
Claims (9)
1. a kind of preparation method of expandable PET resin, it comprises the following steps：
(1) raw material components are mixed evenly；Described raw material components include 985~995 parts of physiochemical mutagens PET bottle piece, expand
1~9 part of chain agent, 1~3 part of antioxidant, 1~3 part of heat stabilizer；Described chain extender by trifunctional chain extension monomer with it is multifunctional
Group's chain extension monomer in mass ratio 1:3~5:1 is compounded, and described trifunctional chain extender is isocyanuric acid three-glycidyl
Ester, described polyfunctional group chain extension monomer are four-functional group chain extender pyromellitic dianhydride and/or six functional groups chain extender
ADR4370；
(2) the material melts extruding pelletization for being well mixed step (1)；
(3) step (2) is granulated obtained material 1~5h of solid phase polycondensation under 210~230 DEG C, 5~100Pa vacuums, obtained
Expandable PET resin.
2. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Described physiochemical mutagens PET bottle
Piece fusing point is 252~256 DEG C, and initial intrinsic viscosity is 0.6~0.7dL/g.
3. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Described physiochemical mutagens PET bottle
Piece pre-processes by drying；Described pretreatment of drying uses following step：First 100~120 DEG C of dryings 10 in convection oven
~15h, is then transferred in vacuum drying oven, 120~150 DEG C of 10~15h of vacuum drying.
4. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Described antioxidant is antioxygen
Agent 1010 and/or irgasfos 168.
5. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Described heat stabilizer is Asia
Triphenyl phosphate and/or triethylene thiophosphoramide.
6. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Described melting extrusion is granulated
Carried out using double screw extruder；One area's temperature of described double screw extruder is 255~275 DEG C, two area's temperature be 255~
275 DEG C, three area's temperature be 260~280 DEG C, four area's temperature are 260~280 DEG C, five area's temperature are 255~275 DEG C, six area's temperature
For 255~275 DEG C；Described double screw extruder feeding machine feeding frequency is 10~20Hz, main frame rotational frequency is 10~
20Hz。
7. the preparation method of expandable PET resin as claimed in claim 1, it is characterised in that：Carrying out described solid phase contracting
Before poly-, first 100~120 DEG C of dry 10~15h in convection oven of described material, it is then transferred in vacuum drying oven, 100~
120 DEG C of 10~15h of vacuum drying.
A kind of 8. expandable PET resin that preparation method as described in any one in claim 1~7 obtains.
9. purposes of the expandable PET resin in PET foamed products as claimed in claim 8.
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| CH713556A1 (en) * | 2017-03-10 | 2018-09-14 | Alpla Werke Alwin Lehner Gmbh & Co Kg | Process for producing a foamed granulate and its use. |
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| CN108976427B (en) * | 2018-07-04 | 2021-06-04 | 华东理工大学 | Modified resin, raw material composition, preparation method, foaming material and application |
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