CN103044869B - Fire-retardant enhancing pet material of high crystallization rate and preparation method thereof - Google Patents
Fire-retardant enhancing pet material of high crystallization rate and preparation method thereof Download PDFInfo
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- CN103044869B CN103044869B CN201310028779.3A CN201310028779A CN103044869B CN 103044869 B CN103044869 B CN 103044869B CN 201310028779 A CN201310028779 A CN 201310028779A CN 103044869 B CN103044869 B CN 103044869B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92885—Screw or gear
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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Abstract
Invention relates to fire-retardant enhancing pet material of a kind of high crystallization rate and preparation method thereof, and product is applicable to the manufacture of electronic apparatus shell, electric appliance and electronic junctor, spark coil, electric and electronic rly. etc.Its component is: PET resin 30.0 ~ 60.0wt%; Reinforcing filler 30.0 ~ 55.0wt%; Fire retardant 1.0 ~ 15.0wt%; Nucleator 0.1 ~ 5.0wt%; Lubricant 0.1 ~ 5.0wt%; Oxidation inhibitor 0.1 ~ 5.0wt%; Described reinforcing filler is glass fibre.It is reasonable that the present invention has formulating of recipe, and product has the advantage of high crystallization rate, good injection molding performance and mechanical property.
Description
Technical field
The present invention relates to fire-retardant enhancing pet material of a kind of high crystallization rate and preparation method thereof, product is applicable to the manufacture of electronic apparatus shell, electric appliance and electronic junctor, spark coil, electric and electronic rly. etc.
Background technology
PET is highly crystalline polymkeric substance, surface smoothing gloss.There is good resistance to creep, fatigue resistance, rub resistance are good, wear away little and hardness is high; Electrical insulation properties is good, nontoxic, weathering resistance, chemical proof good stability, water-intake rate is low, the advantage of weak acid resistant and organic solvent, especially PET institute spent glycol is produced than the price almost cheap half of producing PBT butyleneglycol used, so PET resin and REINFORCED PET are that in engineering plastics, price is minimum, there is very high cost performance.
But the second-order transition temperature of PET resin is higher, crystallization velocity is slow, molding cycle is long, shaping cycle is long, and molding shrinkage is large, poor dimensional stability, the shaping of crystallization is fragility, the deficiency of the low grade of thermotolerance significantly limit the Application Areas of PET as engineering plastics, is maximumly at present applied as fibrous woven and food product pack, is far from playing the value of PET as a engineering plastics of good performance.Be nucleator with nano-calcium carbonate in patent CN 1789329A high-performance refractory reinforced polyester (PET) engineering materials, by each component cooperation, above solve the precipitation of common flame-retardant reinforced polyester fire retardant high temperature, glass fibre exposes, shaping cycle is grown, a difficult problem of Mo Wengao; Patent CN1990514A is used for core-shell structure ionomer of PET resin toughening crystallization and preparation method thereof, serves object that is toughness reinforcing and promotion crystallization, and maintains the price advantage of PET, widened the Application Areas of PET in engineering plastics to PET.In patent CN101440203A a kind of environmental protection flame retardant strengthen in pet resin composition and method of making the same describe that a kind of fire-retardant thermotolerance reaching UL-94 V-0 level is better, rigidity better, the PET engineering plastics preparation method of good stability of the dimension.Organic RE phosphate ester salt is adopted to prepare halogen-free flameproof as nucleator in patent CN101445650A halogen-free flameproof ethylene glycol terephthalate engineering plastic composite material and preparation method thereof, crystallization velocity is fast, good fluidity, high comprehensive performance have the PET engineering plastics of environment friendly concurrently, and performance can be suitable with the FR530 performance of Du Pont.In addition, by research crystallization nucleating agent to the promoter action of PET crystallization, or introducing has more flexible segment reduction PET molecule chain rigidity to improve the method for its molecular motion activity in PET molecule segment, the crystallization rate of PET effectively can be improved under the prerequisite not reducing PET various aspects of performance, PET is made to become one of most engineering plastics having cost performance, become the hot fields of current research, and obtaining section divides achievement.
In sum, PET has caused the extensive common recognition in industry as the potential using value of engineering plastics, wish successfully to include PET in engineering plastics cited field by each side research, but at present in PET research, ubiquity complicated process of preparation, crystallization rate are comparatively slow, cost is higher, be difficult to ensure that material various aspects of performance is all more outstanding, be the feature that partial properties increases, have impact on the large-scale promotion application of PET as engineering plastics.So the novel method of inventing simple, the effective modified PET of a kind of technology of preparing becomes problem demanding prompt solution.(herein, can these several patents, supplement the scheme relative to us, their respective shortcoming, ubiquitous shortcoming in other words)
Summary of the invention
It is reasonable that technical problem to be solved by this invention is to provide a kind of formulating of recipe, and product has the fire-retardant enhancing pet material of high crystallization rate of high crystallization rate, good injection molding performance and mechanical property.
Another technical problem to be solved by this invention be to provide a kind of technological design rationally, the preparation method of the fire-retardant enhancing pet material of high crystallization rate of good product performance.
It is the fire-retardant enhancing pet material of this high crystallization rate that the present invention solves the problems of the technologies described above adopted technical scheme, and its component is:
PET resin 30.0 ~ 60.0wt%
Reinforcing filler 30.0 ~ 55.0wt%
Fire retardant 1.0 ~ 15.0wt%
Nucleator 0.1 ~ 5.0 wt%
Lubricant 0.1 ~ 5.0 wt%
Oxidation inhibitor 0.1 ~ 5.0 wt%;
Described reinforcing filler is glass fibre.
As preferably, component of the present invention is:
PET resin 40.0 ~ 60.0wt%
Reinforcing filler 30.0 ~ 50.0wt%
Fire retardant 1.0 ~ 15.0wt%
Nucleator 0.1 ~ 1.7wt%
Lubricant 0.1 ~ 1.7 wt%
Oxidation inhibitor 0.1 ~ 0.6 wt%.
More than fill a prescription, improve the high-speed crystallization performance of product further comprehensively, flame retardant properties, to strengthen the property.The consumption of nucleator greatly reduces, and under the prerequisite of retention, can reduce costs greatly.The reduction of reinforcing filler content, on the basis keeping mechanical property, can improve the surface property of material, have surface brighter and cleaner, attractive in appearance.
As preferably, PET resin range of viscosities of the present invention, within the scope of 0.55dl/g ~ 1.0dl/g, is one or more in bright chip, semi-dulling chips, full-dull polyester.
As preferably, strongthener of the present invention is glass fibre or inorganic powder strongthener, described glass fibre length-to-diameter ratio >=20:1, and diameter is within the scope of 5 ~ 20um; Inorganic powder strongthener particle diameter is 200 order ~ 4000 order scopes.
As preferably, fire retardant of the present invention is have one or more in halogen fire retardant, halogen-free flame retardants and fire retarding synergist thereof, its fire retardant is halogenated flame retardant or nitrogen, phosphorus flame retardant, be specially brominated Polystyrene/antimonous oxide, TDE/sodium antimoniate, brominated polystyrene/antimonous oxide, melamine cyanurate, one or more in solid phosphate ester, melamine phosphate, hypophosphite or red phosphor masterbatch.
As preferably, nucleator of the present invention be in metal salt of organic carboxylic acid, nanomete talc powder, sodium-based montmorillonite any one or composite, lubricant is pentaerythritol stearate and/or Zinic stearas.
The composite use of above-mentioned preferred nucleator and lubricant, especially has fabulous performance in release property improving nucleation and crystallization, processibility.Make product actual, to make housing of mini-type circuit breaker, under identical Shooting Technique condition, shaping cycle is substantially suitable with nylon material, and compared with DuPont material FR530 NC010 of the same type, its demolding performace is more excellent.And better maintain the mechanical property of material, and under same test condition, creep resistance is substantially suitable with FR530 NC010.
As preferably, metal salt of organic carboxylic acid of the present invention is one or more in Sodium Benzoate, benzoate, unary carboxylation, aromatic phosphoric acid salt, poly-(alkylene terephthalate) or aromatic sulphonate.
Nucleator of the present invention is in inorganic nucleator and/or organic nucleating agent, is specially one or more in small molecule organic compound, sarin resin, silicon-dioxide, silicate, calcium carbonate or wollastonite.
Nucleator is the high crystallization rate nucleator of a kind of promotion, and being not limited to above material, can also be that some has the organism of crystallization nucleation promoter action.
Lubricant of the present invention is fatty amide, calcium stearate, one or more in inspissated wax, polyethylene wax.
As preferably; oxidation inhibitor of the present invention preferably N; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester, one in two (2,4-di-t-butyl) season tetrol diphosphites or two kinds.
Two kinds of oxidation inhibitor can be used composite, and one is primary antioxidant, and one is auxiliary antioxidant, and the ratio of primary antioxidant and auxiliary antioxidant is preferably 1:1.UV resistant and anti-aging in there is extraordinary performance.
The quickening of crystallization rate of the present invention, by improving crystallization onset temperature, crystallization end temp, reduces second-order transition temperature, shortens crystallization time on the one hand, realizes its rapid crystallization at high temperature on the other hand as far as possible and realizes.Tc is between 190 DEG C ~ 230 DEG C.
The present invention solves the problems of the technologies described above the preparation method of adopted technical scheme or the fire-retardant enhancing pet material of a kind of high crystallization rate, and its preparation process is:
A, get PET resin and related auxiliaries, reinforcing filler, fire retardant, nucleator, lubricant, oxidation inhibitor and auxiliary agent;
B, PET resin and related auxiliaries hand mix is even, add at main spout; Reinforcing filler adds at side spout;
C, to be mixed on the twin screw extruder by the material mixed and extrude, its temperature is set to: a district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C.
D, through extruding, pelletizing, drying for standby, completes whole operation.
The present invention compares with existing technology, has the following advantages and feature:
For the feature that PET crystallization velocity is slower, by adding a kind of single-component or composite polycomponent PET crystallization promotion nucleator, with particular lubricants with the use of, by the promotion nucleation and crystallization effect of nucleator in PET, first by the first principles analysis to PET crystallization nucleation, binding tests is verified, the high crystallization rate and the flame retardant resistance that achieve polyethylene terephthalate (PET) material strengthen.This product is suitable with Du Pont analogous products FR530 performance in performance, but processing release property is better than Du Pont analogous products FR530.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1
Take 10g Sodium Benzoate, the nanomete talc powder of 5g, mixes, and makes 15g nucleator.
Take the PET bright chip that 1638g viscosity is 0.78 ± 0.02dl/g, 15g nucleator, 15g lubricant silicone powder, oxidation inhibitor four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 6g(is 12g altogether, account for gross weight 0.4%), 420g brominated Polystyrene and synergist antimonous oxide (commercially available) thereof, mix, add at extruder main spout, 900g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table one.
Embodiment 2
Take nanomete talc powder, each 10g of sodium-based montmorillonite, benzoate 15g, mixes, and makes 35g nucleator.
Take PET bright chip that 1482g viscosity is 0.65 ± 0.02dl/g, 35g nucleator, 25g lubricant fatty amide, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 4g, 400g brominated epoxy resin/synergist sodium antimoniate (commercially available), mix, add at extruder main spout, 1050g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table one.
Embodiment 3
Take 10g poly-(alkylene terephthalate), the nano-calcium carbonate of 10g, mixes, and makes 20g nucleator.
Take PET bright chip that 1388g viscosity is 0.78 ± 0.02dl/g, 20g nucleator, 18g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 7g, 360g solid phosphate ester (commercially available), mix, add at extruder main spout, 1200g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table one.
Embodiment 4
Take 10g sarin resin, 5g silicon-dioxide, the nano-calcium carbonate of 10g, mixes, and makes 25g nucleator.
Take PET semi-dulling chips, 25g nucleator, 15g lubricant silicone powder, N that 1330g viscosity is 0.80 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 6g, 268g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at extruder main spout; 1350g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table one.
Embodiment 5
Take 2g talcum powder, 5g sodium-based montmorillonite, mixes, and makes 7g nucleator.
Take PET bright chip, 7g nucleator, 12g lubricant stearic acid zinc, N that 1200g viscosity is 0.85 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 3g, 278g flame-retardants melamine phosphoric acid salt (commercially available); mix; add at extruder main spout; 1500g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table one.
Comparative example
According to example one, I is taken charge of material and under identical Shooting Technique condition, make sample with Du Pont material of the same type FR530 NC010, according to phase standard, performance test is carried out to sample.Specific performance is in table one.
Table one
Note: comparative example shown in table one is Du Pont like product FR530 NC010 measured performance.
Embodiment 6
Take 100g aromatic phosphoric acid salt, the sodium-based montmorillonite of 50g, mixes, and makes 150g nucleator.
Take PET bright chip, 150g nucleator, 90g lubricant silicone powder, oxidation inhibitor N that 1500g viscosity is 0.78 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 30g, 300g brominated Polystyrene and synergist antimonous oxide (commercially available) thereof; mix; add at extruder main spout; 900g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table two.
Embodiment 7
Take nanomete talc powder, sodium-based montmorillonite, each 3g of benzoate, mix, make 9g nucleator.
Take PET bright chip that 1800g viscosity is 0.65 ± 0.02dl/g, 9g nucleator, 3g lubricant fatty amide, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 1.5g, 150g brominated epoxy resin/synergist sodium antimoniate (commercially available), mix, add at extruder main spout, 1035g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table two.
Embodiment 8
Take 80g poly-(alkylene terephthalate), the nano-calcium carbonate of 40g, mixes, and makes 120g nucleator.
Take PET bright chip that 1050g viscosity is 0.78 ± 0.02dl/g, 120g nucleator, 30g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 2g, 360g solid phosphate ester (commercially available), mix, add at extruder main spout, 1320g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table two.
Embodiment 9
Take 10g sarin resin, 30g silicon-dioxide, the nano-calcium carbonate of 11g, mixes, and makes 51g nucleator.
Take PET semi-dulling chips, 51g nucleator, 60g lubricant silicone powder, N that 1740g viscosity is 0.80 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 45g, 90g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at extruder main spout; 969g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table two.
Embodiment 10
Take 15g talcum powder, 15g sodium-based montmorillonite, 15g unary carboxylation, mixes, and makes 45g nucleator.
Take PET bright chip, 45g nucleator, 120g lubricant stearic acid zinc, N that 900g viscosity is 0.85 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098) 55g, two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) 50g, 180g flame-retardants melamine phosphoric acid salt (commercially available); mix; add at extruder main spout; 1650g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table two.
Table two
Note: comparative example shown in table two is Du Pont like product FR530 NC010 measured performance.
Embodiment 11
Take 50g Sodium Benzoate, the nanomete talc powder of 40g, mixes, and makes 90g nucleator.
Take PET bright chip that 1650g viscosity is 0.78 ± 0.02dl/g, 90g nucleator, 75g lubricant inspissated wax, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010) 10g, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) 3.5g, 60g melamine cyanurate (commercially available), mix, add at extruder main spout, 990g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table three.
Embodiment 12
Take nanomete talc powder, sodium-based montmorillonite, each 6g of aromatic sulphonate, mix, make 18g nucleator.
Take PET bright chip, 18g nucleator, 36g lubricant fatty amide, oxidation inhibitor N that 1140g viscosity is 0.98 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 9g, 228g brominated epoxy resin/synergist sodium antimoniate (commercially available); mix; add at extruder main spout; 1560g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table three.
Embodiment 13
Take 2g poly-(alkylene terephthalate), the silicon-dioxide of 1g, mixes, and makes 3g nucleator.
Take PET bright chip, 3g nucleator, 72g lubricant polyethylene wax, oxidation inhibitor N that 1230g viscosity is 0.78 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine 10g, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) 5g, 30g solid phosphate ester (commercially available); mix; add at extruder main spout; 1650g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table three.
Embodiment 14
Take 10g sarin resin, 10g silicon-dioxide, the nano-calcium carbonate of 25g, mixes, and makes 45g nucleator.
Take PET semi-dulling chips, 45g nucleator, 150g lubricant silicone powder, N that 990g viscosity is 0.80 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 22.5g, 270g fire retardant red phosphor masterbatch (commercially available); mix; add at extruder main spout; 1500g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table three.
Embodiment 15
Take 70g talcum powder, 47g sodium-based montmorillonite, mixes, and makes 117g nucleator.
Take PET bright chip, 117g nucleator, 51g lubricant stearic acid zinc, N that 1080g viscosity is 0.85 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 6g, 390g flame-retardants melamine phosphoric acid salt (commercially available); mix; add at extruder main spout; 1350g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table three.
Table three
Note: comparative example shown in table three is Du Pont like product FR530 NC010 measured performance.
Embodiment 16
Take 40g Sodium Benzoate, the nanomete talc powder of 20g, mixes, and makes 60g nucleator.
Take PET bright chip that 1560g viscosity is 0.55 ± 0.02dl/g, 60g nucleator, 48g lubricant silicone powder, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 36g, 120g TDE/sodium antimoniate (commercially available), mix, add at extruder main spout, 1140g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table four.
Embodiment 17
Take nanomete talc powder, sodium-based montmorillonite, each 7g of benzoate, mix, make 21g nucleator.
Take PET bright chip that 1560g viscosity is 0.65 ± 0.02dl/g, 21g nucleator, 24g lubricant fatty amide, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010) 10g, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) 5g, 150g brominated epoxy resin/sodium antimoniate (commercially available), mix, add at extruder main spout, 1230g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table four.
Embodiment 18
Take 30g poly-(alkylene terephthalate), the nano-calcium carbonate of 30g, mixes, and makes 60g nucleator.
Take PET bright chip that 1380g viscosity is 0.78 ± 0.02dl/g, 60g nucleator, 60g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) each 15g, 450g solid phosphate ester (commercially available), mix, add at extruder main spout, 1040g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table four.
Embodiment 19
Take 15g sarin resin, 15g silicon-dioxide, the nano-calcium carbonate of 9g, mixes, and makes 39g nucleator.
Take PET semi-dulling chips, 39g nucleator, 42g lubricant pentaerythritol stearate, N that 999g viscosity is 0.80 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 75g, 330g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at extruder main spout; 1440g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table four.
Embodiment 20
Take 6g talcum powder, 6g sodium-based montmorillonite, mixes, and makes 12g nucleator.
Take PET bright chip, 12g nucleator, 6g lubricant stearic acid zinc, N that 1206g viscosity is 0.95 ± 0.02dl/g; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) each 18g, 210g flame-retardants melamine phosphoric acid salt (commercially available); mix; add at extruder main spout; 1530g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine each district temperature is arranged: a district a: district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C, main frame current value: 20 ~ 40A.Specific performance is in table four.
Table four
Note: comparative example shown in table four is Du Pont like product FR530 NC010 measured performance.
In above-described embodiment, glass fibre length-to-diameter ratio >=20:1, diameter is within the scope of 5 ~ 20um.Particle diameter value 200 order of talcum powder, calcium carbonate, wollastonite, polynite, spherical glass beads, silicon-dioxide etc., to 4000 orders, is generally 400 orders, 800 orders, 1500 orders, 2000 orders, 3000 orders, 4000 orders etc.
Relatively from middle Du Pont like product FR530 NC010 measured performance, the numerical value that the present invention obtains in actual measurement process, limit in view of by surveying instrument, measuring technology level, and different measurement environment, the numerical value that this possibility of result and producer announce has difference.
In addition, it should be noted that, the specific embodiment described in this specification sheets, its formula, title that technique is named etc. can be different.All equivalences of doing according to structure, feature and the principle described in inventional idea of the present invention or simple change, be included in the protection domain of patent of the present invention.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Although the present invention with embodiment openly as above; but it is also not used to limit protection scope of the present invention; any technician being familiar with this technology, not departing from the change and retouching done in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (6)
1. the fire-retardant enhancing pet material of high crystallization rate, its component is:
Described strongthener is glass fibre or inorganic powder strongthener, described nucleator is by inorganic nucleator and organic nucleating agent is composite forms, described inorganic nucleator is one or more in nanomete talc powder, sodium-based montmorillonite, silicon-dioxide, silicate, calcium carbonate or wollastonite, and organic nucleating agent is one or more in Sodium Benzoate, benzoate, unary carboxylation, aromatic phosphoric acid salt, poly-(alkylene terephthalate), sarin resin or aromatic sulphonate;
Described lubricant is one or more in pentaerythritol stearate, Zinic stearas, fatty amide, calcium stearate;
Described oxidation inhibitor is compound antioxidant, and described compound antioxidant is that oxidation inhibitor 1098 is composite by weight 1:1 with oxidation inhibitor S-9228, antioxidant 1010 is composite by weight 1:1 with irgasfos 168,1:1 is composite by weight with irgasfos 168 for oxidation inhibitor 1098;
Described fire retardant is nitrogen, phosphorus flame retardant.
2., according to the fire-retardant enhancing pet material of the high crystallization rate described in claim 1, it is characterized in that, described component is:
3. according to the fire-retardant enhancing pet material of the high crystallization rate described in claim 1, it is characterized in that, described PET resin viscosity is 0.55dl/g ~ 1.0dl/g, is one or more in bright chip, semi-dulling chips, full-dull polyester.
4. according to the fire-retardant enhancing pet material of the high crystallization rate described in claim 1, it is characterized in that, described glass fibre length-to-diameter ratio >=20:1, diameter is within the scope of 5 ~ 20 μm; Inorganic powder strongthener particle diameter is 200 order ~ 4000 order scopes.
5. according to the fire-retardant enhancing pet material of the high crystallization rate described in claim 1, it is characterized in that, described nitrogen, phosphorus flame retardant are selected from one or more in melamine cyanurate, solid phosphate ester, melamine phosphate, hypophosphite or red phosphor masterbatch.
6. the preparation method of the fire-retardant enhancing pet material of the high crystallization rate according to any one of Claims 1 to 5, is characterized in that, comprise the following steps:
A, get PET resin, reinforcing filler, halogen-free flame retardants, composite nucleator, lubricant and oxidation inhibitor; Described strongthener is glass fibre or inorganic powder strongthener; Described halogen-free flame retardants is nitrogen, phosphorus flame retardant; Described composite nucleator is by inorganic nucleator and organic nucleating agent is composite forms, described inorganic nucleator is one or more in nanomete talc powder, sodium-based montmorillonite, silicon-dioxide, silicate, calcium carbonate or wollastonite, and organic nucleating agent is one or more in Sodium Benzoate, benzoate, unary carboxylation, aromatic phosphoric acid salt, poly-(alkylene terephthalate), sarin resin or aromatic sulphonate; Described lubricant is one or more in pentaerythritol stearate, Zinic stearas, fatty amide, calcium stearate; Described oxidation inhibitor is compound antioxidant, and described compound antioxidant is that oxidation inhibitor 1098 is composite by weight 1:1 with oxidation inhibitor S-9228, antioxidant 1010 is composite by weight 1:1 with irgasfos 168,1:1 is composite by weight with irgasfos 168 for oxidation inhibitor 1098;
B, PET resin, halogen-free flame retardants, composite nucleator, lubricant and oxidation inhibitor hand mix is even, add at main spout; Strongthener adds at side spout;
C, to be mixed on the twin screw extruder by the material mixed and extrude, its temperature is set to: a district: 260 DEG C, 2nd district: 260 DEG C, 3rd district: 260 DEG C, 4th district: 260 DEG C, 5th district: 250 DEG C, 6th district: 220 DEG C, 7th district: 220 DEG C, 8th district: 220 DEG C, 9th district: 220 DEG C, head: 265 DEG C.
D, through extruding, pelletizing, drying for standby, complete whole operation.
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| CN103214830B (en) * | 2013-04-28 | 2015-05-06 | 合肥工业大学 | Preparation method of high-strength and high-toughness polyamide/polyester alloy |
| CN104177787A (en) * | 2013-05-24 | 2014-12-03 | 上海杰事杰新材料(集团)股份有限公司 | Low shrinkage and high strength modified PET (polyethylene terephthalate) material and preparation method thereof |
| CN103265794A (en) * | 2013-05-31 | 2013-08-28 | 常熟市弘基无纺制品有限公司 | Method for preparing environmentally-friendly polyethylene terephthalate molding compound |
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| CN105176010A (en) * | 2014-06-09 | 2015-12-23 | 南通慧源塑胶有限公司 | Improved polyethylene terephthalate formula |
| CN104312110A (en) * | 2014-10-21 | 2015-01-28 | 金宝丽科技（苏州）有限公司 | Composite reinforced PET material |
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| CN106117990A (en) * | 2016-07-04 | 2016-11-16 | 安徽祈艾特电子科技股份有限公司 | A kind of highly crystalline speed PBT material with epoxy bond and preparation method thereof |
| CN109423017A (en) * | 2017-08-29 | 2019-03-05 | 合肥杰事杰新材料股份有限公司 | A kind of PET composition and preparation method thereof |
| CN109721971A (en) * | 2019-01-22 | 2019-05-07 | 江苏博云塑业股份有限公司 | A kind of REINFORCED PET engineering plastics of rapid crystallization and preparation method thereof |
| CN110358269A (en) * | 2019-07-31 | 2019-10-22 | 广东美的厨房电器制造有限公司 | Electric elements plastics composite, plastics and its preparation method and application and electric elements |
| CN112694721A (en) * | 2020-12-25 | 2021-04-23 | 青岛中新华美塑料有限公司 | High-flame-retardant high-glow-wire glass fiber reinforced polyethylene terephthalate material and preparation method thereof |
| CN115093682B (en) * | 2022-07-25 | 2024-04-09 | 宁波华腾首研新材料有限公司 | Glass fiber reinforced PET composite material and preparation method thereof |
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