CN106380799A - Preparation method of flame-retardant and high-heat-resisting polyethylene terephthalate - Google Patents
Preparation method of flame-retardant and high-heat-resisting polyethylene terephthalate Download PDFInfo
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- CN106380799A CN106380799A CN201610839709.XA CN201610839709A CN106380799A CN 106380799 A CN106380799 A CN 106380799A CN 201610839709 A CN201610839709 A CN 201610839709A CN 106380799 A CN106380799 A CN 106380799A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Abstract
The invention discloses a preparation method of flame-retardant and high-heat-resisting polyethylene terephthalate. The preparation method is characterized by comprising the following steps: drying raw materials; uniformly mixing the dried raw material, namely polyethylene terephthalate aggregates, a blended polymer, a nucleating agent, a chain extender, a fire retardant, a stabilizer, a hydrolysis resisting agent and a lubricating agent; adding a mixed material into a double-screw extruder; performing melting extrusion, cooling, dicing and drying, thus obtaining the lame-retardant and high-heat-resisting polyethylene terephthalate with the characteristics of good heat resistance, mechanical property and processing performance; a sheet obtained by compression moulding forming of master batches or a coiled material obtained by a flow casting method can be continuously used at the high temperature of 240DEG C for 30 minutes. The PET master batches obtained by the preparation method disclosed by the invention can be processed into forms such as fibers, fabrics, thin films and sheets, replaces traditional PET and CPET for being applied to the fields with higher heat resisting requirements, such as aviation meal boxes, or can replace nylon with high cost.
Description
Technical field
The invention belongs to the preparation of macromolecular material, it is related to a kind of fire-retardant, high heat-resisting polyethylene terephthalate
Preparation method, particularly to a kind of preparation method of modified polyethylene terephthalate.The product of present invention preparation removes
Possess outside common polyethylene terephthalate (abbreviation PET) excellent mechanics, solvent resistant and the performance such as nontoxic, in processing
In the case that performance is uninfluenced, heat resistance also significantly improves, or even is higher than crystal type PET (abbreviation CPET).Therefore, the present invention
Fire-retardant, the high heat-resisting polyethylene terephthalate product of preparation can be processed into the forms such as fiber, fabric, film, sheet material,
Substitute traditional PET and CPET and be used for the higher field of heat resistant requirements.
Background technology
Polyethylene terephthalate (abbreviation PET) has good chemicals-resistant, creep resistance and the Optimality such as heat-resisting
Can, there is within the scope of wider temperature excellent physical and mechanical properties, Long-Time Service temperature is up to 120 DEG C, and price phase
To cheap, easy recovery, fiber, film and plastic products have been widely used as it.Especially, there is the CPET of high-crystallinity,
Further shorten the PET process-cycle, improve the maximum operation (service) temperature of PET, widen the application of PET.But existing skill
In art, through the modified CPET of nucleation, even the PET of glass fiber reinforcement, their maximum operation (service) temperature is still limited in 220
Within DEG C.And, the candle wick effect due to glass fibre, there is the defect of poor flame retardant properties in its enhanced PET, high crystallinity
Also make the toughness of CPET poor.Due to disadvantages described above, at present existing PET cannot meet under some special dimensions and environment should
Use demand.
Content of the invention
The purpose of the present invention is intended to overcome deficiency of the prior art, provides a kind of fire-retardant, high heat-resisting poly terephthalic acid
The preparation method of glycol ester.Thus provide a kind of use temperature to reach the standard grade more than 220 DEG C and have higher toughness fire-retardant,
The preparation method of high heat-resisting polyethylene terephthalate.
Present disclosure is：A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, is characterized in that
Step is：
A, pretreatment of raw material：
By raw material polyethylene terephthalate (abbreviation PET) pellet, blending macromolecule in 120 DEG C～140 DEG C temperature
Lower drying 3～5 hours, by raw material nucleator, chain extender, fire retardant, stabilizer, hydrolysis-resisting agent at a temperature of 100 DEG C～130 DEG C
It is dried 2～4 hours, take lubricant stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 60～90 mass parts, blending macromolecule 0～40 matter
Amount part, nucleator 0～5 mass parts, chain extender 0～10 mass parts, fire retardant 0.1～5 mass parts, stabilizer 0～5 mass parts,
Hydrolysis-resisting agent 0～10 mass parts, lubricant 0～5 mass parts, whole raw materials are mixed, obtain compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant for heat decomposition temperature
Any one in FR-104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in stirring in high-speed mixer, and (speed of agitator of this high-speed mixer can be 700～1500r/
Min) after mixing 5～10min, add mixture into double screw extruder charging hopper, be 40～100r/ in rate of feeding
Min, screw speed are for 80～400r/min (i.e.：Rev/min) and processing temperature be 230～280 DEG C under conditions of, will mix
Material carries out melting, extrudes, then after supercooling, pelletizing, pellet is dried 1～4h at a temperature of 100～120 DEG C, that is, be obtained fire-retardant,
High heat-resisting polyethylene terephthalate (or claiming modified polyethylene terephthalate) (master batch).
In present disclosure：Described in step b, dispensing is preferably：Take dried raw material polyethylene terephthalate
Ester pellet 60～90 mass parts, blending macromolecule 0～40 mass parts, nucleator 0.1～5 mass parts, chain extender 0～10 mass
Part, fire retardant 0.1～5 mass parts, stabilizer 0.1～5 mass parts, hydrolysis-resisting agent 0.1～10 mass parts, lubricant 0.1～5 matter
Amount part, whole raw materials is mixed, obtains compound.
In present disclosure：Described in step b, dispensing is preferably：Take dried raw material polyethylene terephthalate
Ester pellet 60～90 mass parts, blending macromolecule 0.1～40 mass parts, nucleator 0.1～5 mass parts, chain extender 0.1～10 matter
Amount part, fire retardant 0.1～5 mass parts, stabilizer 0.1～5 mass parts, hydrolysis-resisting agent 0.1～10 mass parts, lubricant 0.1～5
Mass parts, whole raw materials are mixed, obtain compound.
In present disclosure：Polyethylene terephthalate pellet described in step a can be Du Pont 56151, on
Any one in the Hai Yuanfang cb602 and general assorted WP56151 in Sichuan.
In present disclosure：Blending macromolecule described in step a can be polyphenylene sulfide (abbreviation PPS) (production
Enterprise and trade name and model have：Chevron Corporation Philips/R4-XT, U.S.'s Ticona/1140L6, toray/
A360MB etc.), (production enterprise and trade name and model have Merlon (abbreviation PC)：Japanese Supreme Being people/Panlite L-
1225L, Bayer Bitterfeld GmbH/6870, Japan go out light/LC1500 etc.) and nylon66 fiber (production enterprise and trade name and type
Number have：German BASF/A3SK, Dupont/101L, French sieve ground Asia/A205F etc.) in any one.
In present disclosure：Nucleator described in step a can (production enterprise has for nano-attapulgite：Anhui
Province Ming Mei mineral Chemical Co., Ltd., Jiangsu nine river nano material Co., Ltd, Changzhou One Dimension Nanometer Material Technology Co. Ltd
Deng), (production enterprise and model have rutile TiO_2：Sichuan Zhong Kebei Tener rice Science and Technology Ltd. A101, Du Pont's titanium
White powder R-706, Panzhihua big intercommunication Tai Ye Co., Ltd HTR-616 etc.), (production enterprise and model have nano-MgO：Mountain
West Asia emerging magnesia factory, Shanghai Xiang Tian nano material Co., Ltd XT-0806-4), (Dongguan three combination work has nucleant agent N u606
Limit company produces to be provided) and BRUGGOLEN P250 (German Brueggemann produce provide) in any one.
In present disclosure：Chain extender described in step a can for anhydrides (production enterprise and trade name and
Model has：Holland of Zhengzhou Zhi Yuan chemical products Co., Ltd DSM succinic anhydride, the Regratex of Italian POLICHEM company
MB-D), (production enterprise and trade name and model have epoxy resin：Guangzhou Yuan Tai synthetic material Co., Ltd YTPA-
801st, the SAG-008 of Yuyao City monic Chemical Co., Ltd. REPAIPTM CE-3, Jia Yirong compatilizer Co., Ltd, Nanjing good fortune
Poly- Chemical Co., Ltd. ESC-LP-5200 etc.) and cyanate (production enterprise and model have：Shanghai Hua Honghai chemical industry has
Limit company BADCy) in any one.
In present disclosure：Lubricant described in step a can for pentaerythritol stearate (production enterprise and
Model has：Dongguan mountain one plastify Co., Ltd PETS), (production enterprise and model have Tissuemat E：U.S. Honeywell
AC6A) and ethylene bis stearamide (production enterprise and model have：Korea S cell EBS) in any one.
In present disclosure：Hydrolysis-resisting agent described in step a can be gathering that Shanghai You En Chemical Co., Ltd. provides
Carbodiimides UN-03, Rhein chemistry Stabaxol P200 and German Raschig N, N- bis- (2,6- diisopropyl benzenes
Base) any one in carbodiimide (abbreviation R-7000).
In present disclosure：Stabilizer described in step a (or antioxidant) can be called：N, N'- pair-(3- (3,5- bis-
Tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine (abbreviation antioxidant 1098, BASF, vapour bar), four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester (abbreviation antioxidant 1010) and three (2,4- di-tert-butyl-phenyl) phosphorous acid
Any one in ester (abbreviation irgasfos 168, BASF, vapour bar).
Compared with prior art, the present invention has following features and beneficial effect：
(1) adopt the present invention, using the synergistic effect of induction crystallization, chain extension and blending and modifying, obtain and be resistant to 240 DEG C of high temperature
PET；The addition of nucleator, there is heterogeneous nucleation in induction PET, improve the degree of crystallinity of PET；Functional group in chain extender and PET
The carboxyl of end group or hydroxyl reaction, make PET molecular weight increase；The increase of the raising of degree of crystallinity and molecular weight is all conducive to improving
The heat resistance of PET；Meanwhile, using heat-resist macromolecular material blending and modifying PET, it is possible to obtain heat resistance is purer
The high polymer alloy of PET；
(2) adopt the present invention, due to the induction nucleation of inorganic nucleator, the thickening of chain extender and high molecular induction nucleation
And Modification Effects, thus obtaining all excellent modified PET master batch of heat resistance, mechanical property and processing characteristics；Inorganic nucleator
As heterogeneous nucleation center, the degree of crystallinity of PET can be improved, the intermolecular active force of REINFORCED PET, and then improve the heat-resisting of PET
Property；Chain extender is reacted by the end carboxyl producing or terminal hydroxy group with hydrolysis, and it can will hydrolyze generation as bridge
Small molecule is linked as macromolecular PET again, improves molecular weight and the viscosity of PET, delays PET at high temperature aging；PET is in height
The aging molecular weight causing because of ester linkage hydrolyzing under temperature reduces；Some fusing points macromolecule big compared with PET is it is also possible to as PET
Nuclearing centre, play improve PET degree of crystallinity purpose；In addition, macromolecular material can carry as blending and modifying component
The shock resistance of high PET；It can be seen that, above-mentioned three kinds of modified methods are respectively provided with the effect improving PET heat resistance；The inventive method will
Three kinds of effect synergistics, obtain all excellent modified PET master batch of heat resistance, mechanical property and processing characteristics；
(3) PET master batch that the inventive method is obtained has good anti-flammability (oxygen index (OI) is 33) and processing characteristics, this mother
The sheet material that grain is obtained by compression molding can be persistently using 30min under 240 DEG C of high temperature；The PET master batch that the inventive method obtains
Can be applicable to multiple high temperature resistant occasions, such as Airline meal box, also can replace the nylon of high cost；
(4) adopt the present invention, provide one kind to prepare fire-retardant, high heat-resisting polyethylene terephthalate by physical modification
Method；The present invention has considered induction nucleation, the thickening of chain extender and high molecular induction nucleation and the blending of nucleator
Modifying function, three kinds of effect synergistics, through the control etc. of pretreatment of raw material degree, modifying agent species and expressing technique, preparation
Obtain all excellent modified PET master batch of heat resistance, mechanical property and processing characteristics, this PET master batch safety and environmental protection, have good
Anti-flammability and processing characteristics, this master batch passes through the prepared sheet material of compression molding can be persistently using 30min under 240 DEG C of high temperature
(5) product preparation process of the present invention is simple, easily operates, materials safety environmental protection, nontoxic, not halogen, processing characteristics
Good, low cost, practical.
Brief description
Fig. 1 be the inventive method be obtained PET (A-1) and commercially available CPET (B-1) hot-forming after sheet material (1.1mm) divide
Aging conditions photo not after 220 DEG C (A-2, B-2) and 240 DEG C (A-3, B-3) are heat-treated 30min；This figure explanation：The present invention
The sheet material that the modified PET master batch of embodiment preparation is hot-forming does not have variable color after 220 DEG C and 240 DEG C heat treatment 30min substantially,
Crimp；And the hot-forming sheet material of commercially available CPET master batch has substantially turned to be yellow after 220 DEG C of heat treatment 30min, through 240 DEG C
It is changed into brown after heat treatment 30min, aging obvious；Illustrate preparation method of the present invention for raising PET heat resistance effect is significant.
Specific embodiment
The invention will be further described for example given below plan, but is not to be construed as to the scope of the present invention
Restriction, person skilled in art the present invention is made according to the content of the invention described above some nonessential improve and adjust
Whole, still fall within protection scope of the present invention.
Embodiment 1：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET is placed in 140 DEG C of vacuum drying chambers and is dried 3 hours, by nano-attapulgite, organophosphor
Fire retardant FR -104, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 100r/min, screw rod
Rotating speed is, under conditions of 400r/min and processing temperature are 240 DEG C, compound to be carried out melting, extrudes, then through supercooling,
After pelletizing, pellet is dried 4h at a temperature of 120 DEG C, that is, modified PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting poly terephthalic acid second
Diol ester).
Embodiment 2：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET is placed in 140 DEG C of vacuum drying chambers and is dried 3 hours, by nano-attapulgite, anhydrides
Chain extender MB-D, organophosphorous fire retardant FR-104, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent AC6A premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 40r/min, screw rod
Rotating speed is 400r/min and processing temperature is for, under conditions of 260 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, modified PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting poly terephthalic acid second two
Alcohol ester).
Embodiment 3：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, Merlon (PC) are placed in 140 DEG C of vacuum drying chambers and are dried 3 hours, by nanometer
Concave convex rod, organophosphorous fire retardant FR-104, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent AC6A premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 40r/min, screw rod
Rotating speed is 400r/min and processing temperature is for, under conditions of 260 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, modified PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting poly terephthalic acid second two
Alcohol ester).
Embodiment 4：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, Merlon (PC) are placed in 140 DEG C of vacuum drying chambers and are dried 3 hours, will be organic
Phosphorus fire retardant FR-104, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent AC6A premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 100r/min, screw rod
Rotating speed is 200r/min and processing temperature is for, under conditions of 260 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, modified PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting poly terephthalic acid second two
Alcohol ester).
Embodiment 5：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, polyphenylene sulfide are placed in 120 DEG C of vacuum drying chambers and are dried 5 hours, by rutile-type
TiO2, chain extender ESC-LP-5200, aryl polyphosphonates based flame retardant GP-77, antioxidant 1010 and irgasfos 168 be at 110 DEG C
Lower drying 2 hours；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent Rhein chemistry pressing proportioning weighing in advance
Continue mixing 10min, discharging in high-speed mixer after Stabaxol P200 and lubricant PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 100r/min, screw rod
Rotating speed is 200r/min and processing temperature is for, under conditions of 280 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting polyethylene terephthalate
Ester).
Embodiment 6：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, Merlon are placed in 120 DEG C of vacuum drying chambers and are dried 5 hours, by rutile-type
TiO2, chain extender SAG-008, fire retardant FR 2025, antioxidant 1010 and irgasfos 168 be dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 40r/min, screw rod
Rotating speed is 80r/min and processing temperature is for, under conditions of 250 DEG C, carrying out melting to compound, extruding, through supercooling, pelletizing
Afterwards, pellet is dried 4h at a temperature of 120 DEG C, that is, PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting polyethylene terephthalate).
Embodiment 7：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, nylon66 fiber are placed in 120 DEG C of vacuum drying chambers and are dried 5 hours, by rutile-type
TiO2, chain extender YTPA-801, fire retardant OP1240, antioxidant 1010 and irgasfos 168 be dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent R-7000 pressing proportioning weighing in advance and profit
Continue mixing 10min, discharging in high-speed mixer after lubrication prescription PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 80r/min, screw rod
Rotating speed is 300r/min and processing temperature is for, under conditions of 260 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting polyethylene terephthalate
Ester).
Embodiment 8：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
A, pretreatment of raw material：PET, nylon66 fiber are placed in 120 DEG C of vacuum drying chambers and are dried 5 hours, by nano-MgO, fourth
Dicarboxylic anhydride, fire retardant OP1240, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 80r/min, screw rod
Rotating speed is 300r/min and processing temperature is for, under conditions of 260 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting polyethylene terephthalate
Ester).
Embodiment 9：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Proportioning is raw material components by weight percent：
Step is：
A, pretreatment of raw material：PET, nylon66 fiber are placed in 120 DEG C of vacuum drying chambers and are dried 5 hours, by nano-MgO, cyanogen
Acid esters BADCy, fire retardant OP1240, K30, antioxidant 1010 and irgasfos 168 are dried 2 hours at 110 DEG C；
B, dispensing：Dried material is pressed proportioning weigh, with the hydrolysis-resisting agent UN-03 pressing proportioning weighing in advance and lubrication
Continue mixing 10min, discharging in high-speed mixer after agent PETS premixing；
C, processing：Add mixture into double screw extruder charging hopper；Rate of feeding be 50r/min, screw rod
Rotating speed is 120r/min and processing temperature is for, under conditions of 250 DEG C, carrying out melting to compound, extruding, through supercooling, cut
After grain, pellet is dried 4h at a temperature of 120 DEG C, that is, PET master batch is obtained (i.e.：Fire-retardant, high heat-resisting polyethylene terephthalate
Ester).
The performance of the modified PET material that above-described embodiment is obtained see table：
Embodiment 10：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, step is：
A, pretreatment of raw material：
Raw material polyethylene terephthalate (abbreviation PET) pellet is dried 5 hours at a temperature of 120 DEG C, will be fire-retardant
Agent is dried 4 hours at a temperature of 100 DEG C, takes lubricant stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 60 mass parts fire retardant 0.1 mass parts, will be all
Raw material mixes, and obtains compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant for heat decomposition temperature
Any one in FR-104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in after stirring mixing 5min in high-speed mixer, adds mixture into double screw extruder charging
In funnel, rate of feeding be 40r/min, screw speed be 80r/min (i.e.：Rev/min) and processing temperature be 230 DEG C
Under the conditions of, compound is carried out melting, extrudes, then after supercooling, pelletizing, pellet is dried 4h at a temperature of 100 DEG C, that is, be obtained
Fire-retardant, high heat-resisting polyethylene terephthalate (or claiming modified polyethylene terephthalate) (master batch).
Embodiment 11：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, step is：
A, pretreatment of raw material：
Raw material polyethylene terephthalate (abbreviation PET) pellet, blending macromolecule are dried 3 at a temperature of 140 DEG C
Hour, raw material nucleator, chain extender, fire retardant, stabilizer, hydrolysis-resisting agent are dried 2 hours at a temperature of 130 DEG C, take lubrication
Agent is stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 90 mass parts, blending macromolecule 40 mass parts, one-tenth
Core agent 5 mass parts, chain extender 10 mass parts, fire retardant 5 mass parts, stabilizer 5 mass parts, hydrolysis-resisting agent 10 mass parts, lubrication
Agent 5 mass parts, whole raw materials are mixed, obtain compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant for heat decomposition temperature
Any one in FR-104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in high-speed mixer after stirring mixing 10min, add mixture into double screw extruder plus
In funnel, rate of feeding be 100r/min, screw speed be 400r/min (i.e.：Rev/min) and processing temperature be 280
Under conditions of DEG C, compound is carried out melting, extrudes, then after supercooling, pelletizing, pellet is dried 1h at a temperature of 120 DEG C, that is,
Fire-retardant, high heat-resisting polyethylene terephthalate (or claim modified polyethylene terephthalate) (master batch) is obtained.
Embodiment 12：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, step is：
A, pretreatment of raw material：
Raw material polyethylene terephthalate (abbreviation PET) pellet, blending macromolecule are dried 4 at a temperature of 130 DEG C
Hour, raw material nucleator, chain extender, fire retardant, stabilizer, hydrolysis-resisting agent are dried 3 hours at a temperature of 115 DEG C, take lubrication
Agent is stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 75 mass parts, blending macromolecule 20 mass parts, one-tenth
Core agent 2.5 mass parts, chain extender 5 mass parts, fire retardant 2.6 mass parts, stabilizer 2.5 mass parts, hydrolysis-resisting agent 5 mass parts,
Lubricant 2.5 mass parts, whole raw materials are mixed, obtain compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant for heat decomposition temperature
Any one in FR-104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in after stirring mixing 8min in high-speed mixer, adds mixture into double screw extruder charging
In funnel, rate of feeding be 70r/min, screw speed be 240r/min (i.e.：Rev/min) and processing temperature be 255 DEG C
Under conditions of, compound is carried out melting, extrudes, then after supercooling, pelletizing, pellet is dried 2.5h at a temperature of 110 DEG C, that is,
Fire-retardant, high heat-resisting polyethylene terephthalate (or claim modified polyethylene terephthalate) (master batch) is obtained.
Embodiment 13：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, step is：
A, pretreatment of raw material：
By raw material polyethylene terephthalate (abbreviation PET) pellet, blending macromolecule in 120 DEG C～140 DEG C temperature
Lower drying 3～5 hours, by raw material nucleator, chain extender, fire retardant, stabilizer, hydrolysis-resisting agent at a temperature of 100 DEG C～130 DEG C
It is dried 2～4 hours, take lubricant stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 90 mass parts, blending macromolecule 5 mass parts, nucleation
Agent 2 mass parts, chain extender 3 mass parts, fire retardant 1 mass parts, stabilizer 1 mass parts, hydrolysis-resisting agent 2 mass parts, lubricant 1 matter
Amount part, whole raw materials is mixed, obtains compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant for heat decomposition temperature
Any one in FR-104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in after stirring mixing 5～10min in high-speed mixer, adds mixture into double screw extruder
In charging hopper, rate of feeding be 40～100r/min, screw speed be 80～400r/min (i.e.：Rev/min) and plus
Under conditions of work temperature is 230～280 DEG C, compound is carried out melting, extrudes, then after supercooling, pelletizing, pellet is in 100
1～4h is dried at a temperature of～120 DEG C, that is, be obtained fire-retardant, high heat-resisting polyethylene terephthalate (or claim modified poly- to benzene two
Formic acid glycol ester) (master batch).
Embodiment 14：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 60 mass parts, nucleator
0.1 mass parts, fire retardant 0.1 mass parts, stabilizer 0.1 mass parts, hydrolysis-resisting agent 0.1 mass parts, lubricant 0.1 mass parts,
Whole raw materials are mixed, obtains compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 15：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 90 mass parts, blending high
Molecule 30 mass parts, nucleator 5 mass parts, chain extender 7 mass parts, fire retardant 5 mass parts, stabilizer 5 mass parts, hydrolysis-resisting agent
8 mass parts, lubricant 5 mass parts, whole raw materials are mixed, obtain compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 16：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 75 mass parts, blending high
Molecule 20 mass parts, nucleator 2.5 mass parts, chain extender 4 mass parts, fire retardant 2.5 mass parts, stabilizer 2.5 mass parts, anti-
Hydrolytic reagent 5 mass parts, lubricant 2.5 mass parts, whole raw materials are mixed, obtain compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 17：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 80 mass parts, blending high
Molecule 10 mass parts, nucleator 3 mass parts, chain extender 6 mass parts, fire retardant 2 mass parts, stabilizer 2 mass parts, hydrolysis-resisting agent
4 mass parts, lubricant 1 mass parts, whole raw materials are mixed, obtain compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 18：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 60 mass parts, blending high
Molecule 0.1 mass parts, nucleator 0.1 mass parts, chain extender 0.1 mass parts, fire retardant 0.1 mass parts, stabilizer 0.1 mass
Part, hydrolysis-resisting agent 0.1 mass parts, lubricant 0.1 mass parts, whole raw materials are mixed, obtain compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 19：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet 75 mass parts, blending high
Molecule 20 mass parts, nucleator 2.5 mass parts, chain extender 5 mass parts, fire retardant 2.5 mass parts, stabilizer 2.5 mass parts, anti-
Hydrolytic reagent 5 mass parts, lubricant 2.5 mass parts, whole raw materials are mixed, obtain compound；
Arbitrary in the other the same as in Example 1 0～14, omit.
Embodiment 20～26：
A kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate,
Described in step b, dispensing is：Take dried raw material polyethylene terephthalate pellet (abbreviation PET) 60～90
Mass parts, blending macromolecule 0.1～40 mass parts, nucleator 0.1～5 mass parts, chain extender 0.1～10 mass parts, fire retardant
0.1～5 mass parts, stabilizer 0.1～5 mass parts, hydrolysis-resisting agent 0.1～10 mass parts, lubricant 0.1～5 mass parts, will be complete
Portion's raw material mixes, and obtains compound；
In each embodiment, the concrete mass percent consumption of each raw material of component C see table：
Arbitrary in the other the same as in Example 1 0～14, omit.
In above-described embodiment 10-26：Polyethylene terephthalate pellet described in step a can be Du Pont 56151,
Any one in the far fragrant cb602 and general assorted WP56151 in Sichuan in Shanghai.
In above-described embodiment 10-26：Blending macromolecule described in step a can (product be given birth to for polyphenylene sulfide (abbreviation PPS)
Produce enterprise and trade name and model has：Chevron Corporation Philips/R4-XT, U.S.'s Ticona/1140L6, toray/
A360MB etc.), (production enterprise and trade name and model have Merlon (abbreviation PC)：Japanese Supreme Being people/Panlite L-
1225L, Bayer Bitterfeld GmbH/6870, Japan go out light/LC1500 etc.) and nylon66 fiber (production enterprise and trade name and type
Number have：German BASF/A3SK, Dupont/101L, French sieve ground Asia/A205F etc.) in any one.
In above-described embodiment 10-26：Nucleator described in step a can (production enterprise has for nano-attapulgite：Peace
Emblem province Ming Mei mineral Chemical Co., Ltd., Jiangsu nine river nano material Co., Ltd, the limited public affairs of Changzhou monodimension nanometer material science and technology
Department etc.), (production enterprise and model have rutile TiO_2：Sichuan Zhong Kebei Tener rice Science and Technology Ltd. A101, Du Pont
Titanium dioxide R-706, Panzhihua big intercommunication Tai Ye Co., Ltd HTR-616 etc.), (production enterprise and model have nano-MgO：
Shanxi Ya Xing magnesia factory, Shanghai Xiang Tian nano material Co., Ltd XT-0806-4), nucleant agent N u606 (Dongguan three combination work
Co., Ltd produces to be provided) and BRUGGOLEN P250 (German Brueggemann produce provide) in any one.
In above-described embodiment 10-26：Chain extender described in step a can be anhydrides (production enterprise and trade name
Claim and model has：Holland of Zhengzhou Zhi Yuan chemical products Co., Ltd DSM succinic anhydride, Italian POLICHEM company
Regratex MB-D), (production enterprise and trade name and model have epoxy resin：The Guangzhou source Thailand limited public affairs of synthetic material
Department YTPA-801, the SAG-008 of Yuyao City monic Chemical Co., Ltd. REPAIPTM CE-3, Jia Yirong compatilizer Co., Ltd,
Nanjing Fu Ju Chemical Co., Ltd. ESC-LP-5200 etc.) and cyanate (production enterprise and model have：Shanghai Hua Honghai
Chemical Co., Ltd. BADCy) in any one.
In above-described embodiment 10-26：Lubricant described in step a can (production be looked forward to for pentaerythritol stearate
Industry and model have：Dongguan mountain one plastify Co., Ltd PETS), (production enterprise and model have Tissuemat E：U.S. Huo Niwei
Your AC6A) and ethylene bis stearamide (production enterprise and model have：Korea S cell EBS) in any one.
In above-described embodiment 10-26：Hydrolysis-resisting agent described in step a can provide for Shanghai You En Chemical Co., Ltd.
Polycarbodiimide UN-03, Rhein chemistry Stabaxol P200 and German Raschig N, N- bis- (2,6- diisopropyl benzenes
Base) any one in carbodiimide (abbreviation R-7000).
In above-described embodiment 10-26：Stabilizer described in step a (or antioxidant) can be called：N, N'- pair-(3- (3,
5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine (abbreviation antioxidant 1098, BASF, vapour bar), four [β-(3,5- bis-
Tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (abbreviation antioxidant 1010) and three (2,4- di-tert-butyl-phenyls) are sub-
Any one in phosphate (abbreviation irgasfos 168, BASF, vapour bar).
In above-described embodiment：The each raw material being adopted is commercially available prod.
In above-described embodiment：In the percentage being adopted, not especially indicate, be quality (weight) percentage or
Well known to a person skilled in the art percentage；Described quality (weight) part can be all gram or kilogram.
In above-described embodiment：Technological parameter (temperature, time, speed etc.) in each step and each amounts of components numerical value etc. are
Scope, any point is all applicable.
The technology contents being not specifically delineated in present invention and above-described embodiment are compared with technology.
The invention is not restricted to above-described embodiment, all can implement described in present invention and there is described good result.
Claims (10)
1. a kind of fire-retardant, preparation method of high heat-resisting polyethylene terephthalate, is characterized in that step is：
A, pretreatment of raw material：
Will be little to raw material polyethylene terephthalate pellet, the drying 3 ~ 5 at a temperature of 120 DEG C ~ 140 DEG C of blending macromolecule
When, raw material nucleator, chain extender, fire retardant, stabilizer, hydrolysis-resisting agent are dried at a temperature of 100 DEG C ~ 130 DEG C 2 ~ 4 little
When, take lubricant stand-by；
B, dispensing：
Take dried raw material polyethylene terephthalate pellet 60 ~ 90 mass parts, blending macromolecule 0 ~ 40 mass parts, one-tenth
Core agent 0 ~ 5 mass parts, chain extender 0 ~ 10 mass parts, fire retardant 0.1 ~ 5 mass parts, stabilizer 0 ~ 5 mass parts, hydrolysis-resisting agent 0 ~ 10
Mass parts, lubricant 0 ~ 5 mass parts, whole raw materials are mixed, obtain compound；
Described fire retardant is more than 300 DEG C of Clariant OP1240, U.S. FR2025, organophosphorous fire retardant FR- for heat decomposition temperature
Any one in 104 and aryl polyphosphonates based flame retardant GP-77；
C, processing：
Compound is placed in after stirring mixing 5～10min in high-speed mixer, adds mixture into double screw extruder charging
In funnel, rate of feeding be 40 ~ 100r/min, screw speed be 80 ~ 400r/min and processing temperature be 230 ~ 280 DEG C
Under the conditions of, compound is carried out melting, extrudes, then after supercooling, pelletizing, pellet is dried 1 ~ 4h at a temperature of 100 ~ 120 DEG C,
Fire-retardant, high heat-resisting polyethylene terephthalate is obtained.
2. the preparation method of fire-retardant as described in claim 1, high heat-resisting polyethylene terephthalate, is characterized in that：Step b
Described dispensing is：Take dried raw material polyethylene terephthalate pellet 60 ~ 90 mass parts, blending macromolecule 0 ~ 40 matter
Amount part, nucleator 0.1 ~ 5 mass parts, chain extender 0 ~ 10 mass parts, fire retardant 0.1 ~ 5 mass parts, stabilizer 0.1 ~ 5 mass parts,
Hydrolysis-resisting agent 0.1 ~ 10 mass parts, lubricant 0.1 ~ 5 mass parts, whole raw materials are mixed, obtain compound.
3. the preparation method of fire-retardant as described in claim 2, high heat-resisting polyethylene terephthalate, is characterized in that：Step b
Described dispensing is：Take dried raw material polyethylene terephthalate pellet 60 ~ 90 mass parts, blending macromolecule 0.1 ~ 40
Mass parts, nucleator 0.1 ~ 5 mass parts, chain extender 0.1 ~ 10 mass parts, fire retardant 0.1 ~ 5 mass parts, stabilizer 0.1 ~ 5 mass
Part, hydrolysis-resisting agent 0.1 ~ 10 mass parts, lubricant 0.1 ~ 5 mass parts, whole raw materials are mixed, obtain compound.
4. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
Polyethylene terephthalate pellet described in step a is the far fragrant cb602 in Du Pont 56151, Shanghai and Sichuan is general assorted
Any one in WP56151.
5. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
Blending macromolecule described in step a is any one in polyphenylene sulfide, Merlon and nylon66 fiber.
6. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
Nucleator described in step a is nano-attapulgite, rutile TiO_2, nano-MgO, nucleant agent N u606 and BRUGGOLEN
Any one in P250.
7. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
Chain extender described in step a is any one in acid anhydrides, epoxy resin and cyanate.
8. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
Lubricant described in step a is any one in pentaerythritol stearate, Tissuemat E and ethylene bis stearamide.
9. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, it is characterized in that：
The polycarbodiimide UN-03 that hydrolysis-resisting agent described in step a provides for Shanghai You En Chemical Co., Ltd., Rhein are chemical
Stabaxol P200 and German Raschig N, N- bis-（2,6- diisopropyl phenyls）Any one in carbodiimide.
10. as described in claim 1,2 or 3 fire-retardant, high heat-resisting polyethylene terephthalate preparation method, its feature
It is：Described in step a, stabilizer is：N, N'- be double-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, four
[β-（3,5- di-tert-butyl-hydroxy phenyl）Propionic acid] pentaerythritol ester, Yi Jisan（2,4- di-tert-butyl-phenyl）Phosphite ester
In any one.
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| CN108440924A (en) * | 2018-04-10 | 2018-08-24 | 常州大学 | A kind of polyethylene terephthalate of lighting and preparation method thereof that lazy flow is easy to process |
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| CN108485210A (en) * | 2018-04-09 | 2018-09-04 | 长沙秋点兵信息科技有限公司 | A kind of POF environment-friendlythin thin films and preparation method thereof |
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| CN108641308A (en) * | 2018-04-10 | 2018-10-12 | 温州新鲜源包装材料有限公司 | A kind of PET cutlery boxs formula that heat resistance is high and its manufacturing process |
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| CN109749370A (en) * | 2018-12-21 | 2019-05-14 | 广州华新科智造技术有限公司 | A kind of PET composite nucleating agent and preparation method thereof |
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| CN114479381B (en) * | 2022-03-02 | 2024-01-30 | 无锡会通轻质材料股份有限公司 | Preparation method of PET (polyethylene terephthalate) foaming beads for molding |
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