CN103044869A - High-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material and preparation method thereof - Google Patents
High-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material and preparation method thereof Download PDFInfo
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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
The invention relates to a high-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material and a preparation method thereof. The high-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material is suitable for manufacturing shells of electronic and electrical appliances, electronic connectors of electric appliances, ignition coils, electrical and electronic relays and the like. The high-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material comprises the following components in percentage by weight: 30.0 to 60.0 percent of polyethylene glycol terephthalate (PET) resin, 30.0 to 55.0 percent of reinforcing filler, 1.0 to 15.0 percent of a flame retardant, 0.1 to 5.0 percent of a nucleating agent, 0.1 to 5.0 percent of a lubricant, and 0.1 to 5.0 percent of an antioxidant, wherein the reinforcing filler is glass fiber. The high-crystallization-rate flame-retardant enhanced polyethylene glycol terephthalate material has the advantages of reasonable formula design, high crystallization rate, high injection molding processability and high mechanical properties.
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 manufacturing of electronic apparatus shell, electric appliance and electronic junctor, spark coil, electric and electronic rly. etc.
Background technology
PET is the highly crystalline polymkeric substance, surface smoothing gloss.Have good anti-creep, fatigue resistance, rub resistance 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 produce PET institute spent glycol than the price of producing the used butyleneglycol of PBT almost cheap half, so PET resin and REINFORCED PET are that price is minimum in the engineering plastics, have 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 moulding of crystallization is fragility, the low deficiency that waits of thermotolerance has greatly limited the Application Areas of PET as engineering plastics, maximumly at present is applied as fibrous woven and food product pack, is far from bringing into play PET as the value of a well behaved engineering plastics.In patent CN 1789329A high-performance refractory reinforced polyester (PET) engineering materials take nano-calcium carbonate as nucleator, by each component cooperation, on solved that common flame-retardant reinforced polyester fire retardant high temperature is separated out, glass fibre exposes, shaping cycle is grown, the difficult problem of Mo Wengao; Patent CN1990514A is used for core-shell structure ionomer of PET resin toughening crystallization and preparation method thereof, and PET has been played purpose toughness reinforcing and the promotion crystallization, and has kept the price advantage of PET, has widened the Application Areas of PET in engineering plastics.Among the patent CN101440203A a kind of environmental protection flame retardant strengthen that the thermotolerance of having described a kind of fire-retardant UL-94 of reaching V-0 level in the pet resin composition and method of making the same is better, rigidity better, the PET engineering plastics preparation method of good stability of the dimension.Adopt the organic RE phosphate ester salt 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 the promoter action of research crystallization nucleating agent to the PET crystallization, or in the PET molecule segment, introduce the segment that has more flexibility and reduce the method that PET molecule chain rigidity improves its molecular motion activity, crystallization rate that can Effective Raise PET under the prerequisite that does not reduce the PET various aspects of performance, PET is become have one of engineering plastics of cost performance most, become the hot fields of current research, and obtaining section has been divided achievement.
In sum, PET has caused extensive common recognition in the industry as the potential using value of engineering plastics, hope is successfully included PET in the engineering plastics cited field by each side research, but at present in PET research, ubiquity complicated process of preparation, crystallization rate are slow, cost is higher, being difficult to guarantee that the material various aspects of performance is all more outstanding, is the characteristics that partial properties increases, and has affected the large-scale promotion application of PET as engineering plastics.Become problem demanding prompt solution so invent a kind of technology of preparing novel method simple, effectively modified PET.(herein, can these several patents replenish the scheme with respect to us, they shortcoming separately, in other words ubiquitous shortcoming)
Summary of the invention
It is reasonable that technical problem to be solved by this invention provides a kind of formulating of recipe, and product has high crystallization rate, good injection molding performance and the fire-retardant enhancing pet material of high crystallization rate of mechanical property.
Another technical problem to be solved by this invention 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 the technical scheme that adopts, 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%.
Above prescription has further improved the high speed crystal property of product comprehensively, flame retardant properties, strengthens the property.The consumption of nucleator greatly reduces, and under the prerequisite of retention, can reduce greatly cost.The reduction of reinforcing filler content on the basis that keeps mechanical property, can improve the surface property of material, has surface brighter and cleaner, attractive in appearance.
As preferably, PET resin viscosity scope of the present invention is in 0.55dl/g ~ 1.0dl/g scope, for one or more in light section, semi-dulling chips, the full-dull section are arranged.
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 in 5 ~ 20um scope; Inorganic powder strongthener particle diameter is 200 orders ~ 4000 order scopes.
As preferably, fire retardant of the present invention is one or more that have in halogen fire retardant, halogen-free flame retardants and the 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 the red phosphorus master batch.
As preferably, nucleator of the present invention be in metal salt of organic carboxylic acid, nanomete talc powder, the 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 aspect the release property improving nucleation and crystallization, processibility.At the actual product of making, to make housing of mini-type circuit breaker as example, under identical Shooting Technique condition, shaping cycle is substantially suitable with nylon material, compares with the material FR530 NC010 of Du Pont of the same type, and its demolding performace is more excellent.And better kept the mechanical property of material, and under the 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 the aromatic sulphonate.
Nucleator of the present invention is in inorganic nucleator and/or the organic nucleating agent, is specially in small molecule organic compound, sarin resin, silicon-dioxide, silicate, calcium carbonate or the wollastonite one or more.
Nucleator is the high crystallization rate nucleator of a kind of promotion, is not limited to above material, can also be some organism with crystallization nucleation promoter action.
Lubricant of the present invention is fatty amide, calcium stearate, one or more in inspissated wax, the polyethylene wax.
As preferably; oxidation inhibitor of the present invention is N preferably; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) a kind of in hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester, two (2,4-di-t-butyl) season tetrol diphosphites or two kinds.
Can use two kinds of oxidation inhibitor composite, a kind of is primary antioxidant, and a kind of is auxiliary antioxidant, and the ratio of primary antioxidant and auxiliary antioxidant is preferably 1:1.UV resistant and anti-aging aspect have extraordinary performance.
The quickening of crystallization rate of the present invention reduces second-order transition temperature by improving crystallization onset temperature, crystallization end temp, shortens crystallization time on the one hand, realizes as far as possible that on the other hand its rapid crystallization at high temperature realizes.Tc is between 190 ℃ ~ 230 ℃.
The present invention solves the problems of the technologies described above the technical scheme that adopts or the preparation method of the fire-retardant enhancing pet material of a kind of high crystallization rate, and its preparation process is:
A, get PET resin and relevant auxiliary agent, reinforcing filler, fire retardant, nucleator, lubricant, oxidation inhibitor and auxiliary agent;
B, PET resin and relevant auxiliary agent hand mix is even adds at main spout; Reinforcing filler adds at the side spout;
C, the material that mixes mixed at twin screw extruder extrude, its temperature setting is set to: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃.
D, through extrude, pelletizing, drying for standby is finished whole operation.
The present invention compares with existing technology, has the following advantages and characteristics:
For the slower characteristics of PET crystallization velocity, promote nucleator by adding a kind of single-component or composite polycomponent PET crystallization, be used in conjunction with particular lubricants, by the promotion nucleation and crystallization effect of nucleator in PET, at first by the first principles analysis to the PET crystallization nucleation, in conjunction with verification experimental verification, realized that the high crystallization rate of polyethylene terephthalate (PET) material and flame retardant resistance strengthen.This product is suitable with Du Pont analogous products FR530 performance on performance, but the processing release property is better than the analogous products FR530 of Du Pont.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1
Take by weighing the 10g Sodium Benzoate, the nanomete talc powder of 5g mixes, and makes the 15g nucleator.
The PET that takes by weighing the 1638g viscosity and be 0.78 ± 0.02dl/g has the light section, the 15g nucleator, 15g lubricant silicone powder, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three each 6g(of ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168) are 12g altogether, account for gross weight 0.4%), 420g brominated Polystyrene and synergist antimonous oxide (commercially available) thereof, mix, add at the extruder main spout, 900g glass fibre (commercially available) adds at side spout weight-loss metering, through extruding, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table one.
Embodiment 2
Take by weighing nanomete talc powder, each 10g of sodium-based montmorillonite, benzoate 15g mixes, and makes the 35g nucleator.
The PET that takes by weighing the 1482g viscosity and be 0.65 ± 0.02dl/g has light section, 35g nucleator, 25g lubricant fatty amide, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 4g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 400g brominated epoxy resin/synergist sodium antimoniate (commercially available), mix, add at the extruder main spout, 1050g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table one.
Embodiment 3
Take by weighing 10g poly-(alkylene terephthalate), the nano-calcium carbonate of 10g mixes, and makes the 20g nucleator.
The PET that takes by weighing the 1388g viscosity and be 0.78 ± 0.02dl/g has light section, 20g nucleator, 18g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 7g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 360g solid phosphate ester (commercially available), mix, add at the extruder main spout, 1200g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table one.
Embodiment 4
Take by weighing 10g sarin resin, 5g silicon-dioxide, the nano-calcium carbonate of 10g mixes, and makes the 25g nucleator.
Taking by weighing the 1330g viscosity is PET semi-dulling chips, 25g nucleator, 15g lubricant silicone powder, the N of 0.80 ± 0.02dl/g; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 6g of season tetrol diphosphites (oxidation inhibitor S-9228), 268g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at the extruder main spout; 1350g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table one.
Embodiment 5
Take by weighing the 2g talcum powder, the 5g sodium-based montmorillonite mixes, and makes the 7g nucleator.
The PET that takes by weighing the 1200g viscosity and be 0.85 ± 0.02dl/g has light section, 7g nucleator, 12g lubricant stearic acid zinc, N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 3g of season tetrol diphosphites (oxidation inhibitor S-9228), 278g fire retardant melamine phosphate (commercially available); mix; add at the extruder main spout; 1500g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table one.
Comparative example
According to example one, I am taken charge of material under identical Shooting Technique condition, make sample with the material FR530 of the same type NC010 of Du Pont, according to the phase standard sample is carried out performance test.Specific performance sees Table one.
Table one
Annotate: comparative example shown in the table one is the like product FR530 NC010 of Du Pont measured performance.
Embodiment 6
Take by weighing 100g aromatic phosphoric acid salt, the sodium-based montmorillonite of 50g mixes, and makes the 150g nucleator.
The PET that takes by weighing the 1500g viscosity and be 0.78 ± 0.02dl/g has light section, 150g nucleator, 90g lubricant silicone powder, oxidation inhibitor N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) each 30g of hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 300g brominated Polystyrene and synergist antimonous oxide (commercially available) thereof; mix; add at the extruder main spout; 900g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table two.
Embodiment 7
Take by weighing nanomete talc powder, sodium-based montmorillonite, each 3g of benzoate, mix, make the 9g nucleator.
The PET that takes by weighing the 1800g viscosity and be 0.65 ± 0.02dl/g has light section, 9g nucleator, 3g lubricant fatty amide, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 1.5g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 150g brominated epoxy resin/synergist sodium antimoniate (commercially available), mix, add at the extruder main spout, 1035g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table two.
Embodiment 8
Take by weighing 80g poly-(alkylene terephthalate), the nano-calcium carbonate of 40g mixes, and makes the 120g nucleator.
The PET that takes by weighing the 1050g viscosity and be 0.78 ± 0.02dl/g has light section, 120g nucleator, 30g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 2g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 360g solid phosphate ester (commercially available), mix, add at the extruder main spout, 1320g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table two.
Embodiment 9
Take by weighing 10g sarin resin, 30g silicon-dioxide, the nano-calcium carbonate of 11g mixes, and makes the 51g nucleator.
Taking by weighing the 1740g viscosity is PET semi-dulling chips, 51g nucleator, 60g lubricant silicone powder, the N of 0.80 ± 0.02dl/g; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 45g of season tetrol diphosphites (oxidation inhibitor S-9228), 90g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at the extruder main spout; 969g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table two.
Embodiment 10
Take by weighing the 15g talcum powder, the 15g sodium-based montmorillonite, the 15g unary carboxylation mixes, and makes the 45g nucleator.
The PET that takes by weighing the 900g viscosity and be 0.85 ± 0.02dl/g has light section, 45g nucleator, 120g lubricant stearic acid zinc, N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098) 55g, two (2; the 4-di-t-butyl) season tetrol diphosphites (oxidation inhibitor S-9228) 50g, 180g fire retardant melamine phosphate (commercially available); mix; add at the extruder main spout; 1650g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table two.
Table two
Annotate: comparative example shown in the table two is the like product FR530 NC010 of Du Pont measured performance.
Embodiment 11
Take by weighing the 50g Sodium Benzoate, the nanomete talc powder of 40g mixes, and makes the 90g nucleator.
The PET that takes by weighing the 1650g viscosity and be 0.78 ± 0.02dl/g has light section, 90g nucleator, 75g lubricant inspissated wax, oxidation inhibitor four [β-(3, the 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 the extruder main spout, 990g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table three.
Embodiment 12
Take by weighing nanomete talc powder, sodium-based montmorillonite, each 6g of aromatic sulphonate, mix, make the 18g nucleator.
The PET that takes by weighing the 1140g viscosity and be 0.98 ± 0.02dl/g has light section, 18g nucleator, 36g lubricant fatty amide, oxidation inhibitor N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) each 9g of hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 228g brominated epoxy resin/synergist sodium antimoniate (commercially available); mix; add at the extruder main spout; 1560g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table three.
Embodiment 13
Take by weighing 2g poly-(alkylene terephthalate), the silicon-dioxide of 1g mixes, and makes the 3g nucleator.
The PET that takes by weighing the 1230g viscosity and be 0.78 ± 0.02dl/g has light section, 3g nucleator, 72g lubricant polyethylene wax, oxidation inhibitor N; N'-pair-(3-(3; the 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 the extruder main spout; 1650g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table three.
Embodiment 14
Take by weighing 10g sarin resin, 10g silicon-dioxide, the nano-calcium carbonate of 25g mixes, and makes the 45g nucleator.
Taking by weighing the 990g viscosity is PET semi-dulling chips, 45g nucleator, 150g lubricant silicone powder, the N of 0.80 ± 0.02dl/g; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 22.5g of season tetrol diphosphites (oxidation inhibitor S-9228), 270g fire retardant red phosphorus master batch (commercially available); mix; add at the extruder main spout; 1500g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table three.
Embodiment 15
Take by weighing the 70g talcum powder, the 47g sodium-based montmorillonite mixes, and makes the 117g nucleator.
The PET that takes by weighing the 1080g viscosity and be 0.85 ± 0.02dl/g has light section, 117g nucleator, 51g lubricant stearic acid zinc, N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 6g of season tetrol diphosphites (oxidation inhibitor S-9228), 390g fire retardant melamine phosphate (commercially available); mix; add at the extruder main spout; 1350g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table three.
Table three
Annotate: comparative example shown in the table three is the like product FR530 NC010 of Du Pont measured performance.
Embodiment 16
Take by weighing the 40g Sodium Benzoate, the nanomete talc powder of 20g mixes, and makes the 60g nucleator.
The PET that takes by weighing the 1560g viscosity and be 0.55 ± 0.02dl/g has light section, 60g nucleator, 48g lubricant silicone powder, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 36g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 120g TDE/sodium antimoniate (commercially available), mix, add at the extruder main spout, 1140g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table four.
Embodiment 17
Take by weighing nanomete talc powder, sodium-based montmorillonite, each 7g of benzoate, mix, make the 21g nucleator.
The PET that takes by weighing the 1560g viscosity and be 0.65 ± 0.02dl/g has light section, 21g nucleator, 24g lubricant fatty amide, oxidation inhibitor four [β-(3, the 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 the extruder main spout, 1230g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table four.
Embodiment 18
Take by weighing 30g poly-(alkylene terephthalate), the nano-calcium carbonate of 30g mixes, and makes the 60g nucleator.
The PET that takes by weighing the 1380g viscosity and be 0.78 ± 0.02dl/g has light section, 60g nucleator, 60g lubricant pentaerythritol stearate, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] each 15g of pentaerythritol ester (antioxidant 1010), three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester (irgasfos 168), 450g solid phosphate ester (commercially available), mix, add at the extruder main spout, 1040g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table four.
Embodiment 19
Take by weighing 15g sarin resin, 15g silicon-dioxide, the nano-calcium carbonate of 9g mixes, and makes the 39g nucleator.
Taking by weighing the 999g viscosity is PET semi-dulling chips, 39g nucleator, 42g lubricant pentaerythritol stearate, the N of 0.80 ± 0.02dl/g; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 75g of season tetrol diphosphites (oxidation inhibitor S-9228), 330g fire retardant hypo-aluminum orthophosphate (commercially available); mix; add at the extruder main spout; 1440g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table four.
Embodiment 20
Take by weighing the 6g talcum powder, the 6g sodium-based montmorillonite mixes, and makes the 12g nucleator.
The PET that takes by weighing the 1206g viscosity and be 0.95 ± 0.02dl/g has light section, 12g nucleator, 6g lubricant stearic acid zinc, N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (oxidation inhibitor 1098), two (2; the 4-di-t-butyl) each 18g of season tetrol diphosphites (oxidation inhibitor S-9228), 210g fire retardant melamine phosphate (commercially available); mix; add at the extruder main spout; 1530g glass fibre (commercially available) adds at side spout weight-loss metering, through extrude, pelletizing, for subsequent use.Forcing machine is respectively distinguished the temperature setting: a district: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃, and main frame current value: 20 ~ 40A.Specific performance sees Table four.
Table four
Annotate: comparative example shown in the table four is the like product FR530 NC010 of Du Pont measured performance.
In above-described embodiment, glass fibre length-to-diameter ratio 〉=20:1, diameter is in 5 ~ 20um scope.Particle diameter value 200 orders of talcum powder, calcium carbonate, wollastonite, polynite, spherical glass microballon, silicon-dioxide etc. are generally 400 orders, 800 orders, 1500 orders, 2000 orders, 3000 orders, 4000 orders etc. to 4000 orders.
Relatively from the middle like product FR530 NC010 of Du Pont measured performance, the numerical value that the present invention obtains in the actual measurement process, in view of being limit 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, need to prove, the specific embodiment described in this specification sheets, its prescription, title that technique is named etc. can be different.Allly conceive equivalence or the simple change that described structure, feature and principle are done according to patent of the present invention, be included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Although the present invention with embodiment openly as above; but it is not to limit protection scope of the present invention; any technician who is familiar with this technology not breaking away from change and the retouching of doing in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (10)
1. fire-retardant enhancing pet material of high crystallization rate, 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.
2. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described component 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%.
3. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described PET resin viscosity scope is in 0.55dl/g ~ 1.0dl/g scope, for one or more in light section, semi-dulling chips, the full-dull section are arranged.
4. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described strongthener is glass fibre or inorganic powder strongthener, described glass fibre length-to-diameter ratio 〉=20:1, diameter is in 5 ~ 20um scope; Inorganic powder strongthener particle diameter is 200 orders ~ 4000 order scopes.
5. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described fire retardant is brominated Polystyrene/antimonous oxide, TDE/sodium antimoniate, brominated polystyrene/antimonous oxide, melamine cyanurate, one or more in solid phosphate ester, melamine phosphate, hypophosphite or the red phosphorus master batch.
6. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described nucleator be in metal salt of organic carboxylic acid, nanomete talc powder, the sodium-based montmorillonite any one or composite, lubricant is pentaerythritol stearate and/or Zinic stearas.
7. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 6, it is characterized in that: described metal salt of organic carboxylic acid is one or more in Sodium Benzoate, benzoate, unary carboxylation, aromatic phosphoric acid salt, poly-(alkylene terephthalate) or the aromatic sulphonate.
8. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1, it is characterized in that: described nucleator is in inorganic nucleator and/or the organic nucleating agent, is specially in small molecule organic compound, sarin resin, silicon-dioxide, silicate, calcium carbonate or the wollastonite one or more; Described lubricant is pentaerythritol stearate, Zinic stearas, fatty amide, calcium stearate, one or more in inspissated wax, the polyethylene wax.
9. the fire-retardant enhancing pet material of high crystallization rate described in according to claim 1; it is characterized in that: described oxidation inhibitor is N preferably; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) a kind of in hexanediamine, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester, two (2,4-di-t-butyl) season tetrol diphosphites or two kinds.
10. the preparation method of the fire-retardant enhancing pet material of high crystallization rate according to claim 1 ~ 9, its preparation process is:
A, get PET resin and relevant auxiliary agent, reinforcing filler, fire retardant, nucleator, lubricant and oxidation inhibitor;
B, PET resin and relevant auxiliary agent hand mix is even adds at main spout; Reinforcing filler adds at the side spout;
C, the material that mixes mixed at twin screw extruder extrude, its temperature setting is set to: a district: 260 ℃, two districts: 260 ℃, three districts: 260 ℃, four districts: 260 ℃, five districts: 250 ℃, six districts: 220 ℃, seven districts: 220 ℃, eight districts: 220 ℃, nine districts: 220 ℃, head: 265 ℃;
D, through extrude, pelletizing, drying for standby is finished whole operation.
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| 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 |
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