CN104419195A - Inorganic mineral filled semi-aromatic nylon composite material and preparation method thereof - Google Patents

Inorganic mineral filled semi-aromatic nylon composite material and preparation method thereof Download PDF

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Publication number
CN104419195A
CN104419195A CN201310368483.6A CN201310368483A CN104419195A CN 104419195 A CN104419195 A CN 104419195A CN 201310368483 A CN201310368483 A CN 201310368483A CN 104419195 A CN104419195 A CN 104419195A
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temperature
district
semi
parts
aromatic nylon
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杨桂生
李宗仁
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Shanghai Genius Advanced Materials Group Co Ltd
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Shanghai Genius Advanced Materials Group Co Ltd
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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
    • 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
    • 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
    • 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
    • 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
    • C08K5/54—Silicon-containing compounds
    • C08K5/544—Silicon-containing compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • 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
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • 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
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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

Abstract

The invention belongs to the technical fields of high-molecular material processing and modification, and relates to an inorganic mineral filled semi-aromatic nylon composite material and a preparation method thereof. The composite material is prepared by using the following components, by weight, 60-90 parts of semi-aromatic nylon resin, 10-40 parts of an inorganic mineral filler, 5-10 parts of a compatilizer, 0.5-2 parts of an antioxidant, 0.3-1 part of a coupling agent and 1-3 parts of a lubricant. The semi-aromatic nylon composite material has the advantages of excellent heat resistance, good apparent quality, high rigidity and workability.

Description

A kind of inorganic mineral fills semi-aromatic nylon composite and preparation method thereof
Technical field
The invention belongs to processing of high molecular material and technical field of modification, relate to a kind of semi-aromatic nylon composite and preparation method thereof.
Background technology
Semi-aromatic nylon is the diacid or the diamines that have aliphatie diamine or diacid and band aromatic nucleus, obtains through polycondensation, is the one of aromatic nylon.Owing to introducing aromatic ring structure in the main chain of nylon molecules, thus the resistance toheat of nylon product and mechanical property are greatly improved, water-intake rate also has reduction in various degree simultaneously, and there is higher cost performance, be the high heat resistance resin material between general engineering plastic and thermostability engineering plastic PEEK, be mainly used in automobile and electric and electronic industry.Because semi-aromatic nylon is compared with nylon66 fiber, its maximum feature is fine heat-resisting performance, low water-intake rate and excellent creep-resistant property; Simultaneously compared with all aromatic nylon, it has the characteristic of easily processing.Therefore, along with the demand with environmental protection cause that develops rapidly of new and high technology, its market requirement is in rising trend, and its application and development also has new progress.
In macromolecular material, add mineral filler is obtain some to have one of approach of the efficient and cost-effective of the high-molecular compounded and modified material of special performance, inorganic mineral filler is the inorganic rigid particle of acid-fast alkali-proof, water insoluble and organic solvent, there is fabulous light stability and weathering resistance, when height is filled, there is fabulous rheological property, wear metal hardly in the course of processing, has been widely used in high-molecular compounded and modified material as inorganic mineral filler.Through the semi-aromatic nylon that inorganic mineral is filling-modified, can significantly improve its intensity, rigidity, mineral-filled semi-aromatic nylon has good apparent mass in addition, and processing characteristics is flowing with great difficulty, the shaping advantage such as soon.
Summary of the invention
The object of the invention is to the defect for overcoming prior art and a kind of semi-aromatic nylon composite and preparation method thereof is provided.
For achieving the above object, the present invention is by the following technical solutions:
In semi-aromatic nylon resin, add inorganic mineral filler carry out modification, provide a kind of simple, with low cost, be applicable to the excellent heat resistance of scale of mass production, high rigidity, the mineral-filled semi-aromatic nylon composite that apparent mass is good.
A kind of semi-aromatic nylon composite, be made up of the component comprising following weight part:
Described semi-aromatic nylon resin be selected from PA4T, PA6T, PA7T, PA8T, PA9T, PA10T, PA12T, PA13T or PA14T one or more, be preferably PA9T, PA10T or PA12T.
Described inorganic mineral filler is one or more in mica, wollastonite, talcum powder, calcium carbonate, barium sulfate or kaolin, preferred wollastonite or kaolin.
Described compatilizer is one or more of maleic anhydride, maleic anhydride-g-SBS, maleic anhydride graft vinylbenzene or maleic anhydride grafted ethene-octene copolymer.
Described oxidation inhibitor phenols high-temperature antioxidant is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid, 1,3,5-tri-(the 4-tertiary butyl-3-hydroxyl-2,6-dimethyl benzyl)-1,3,5-triazines-2,4, one or more in 6-(1H, 3H, 5H)-triketone.
Described coupling agent is the one or more than one in vinyltriethoxysilane, γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, γ-propyl methacrylate base silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, positive titanium isopropylate or the different stearoyl titanic acid ester of sec.-propyl three.Described lubricant is calcium stearate or Zinic stearas.
A preparation method for above-mentioned semi-aromatic nylon composite, comprises the following steps:
(1) first semi-aromatic nylon, inorganic mineral filler are put into respectively loft drier forced air drying for subsequent use;
(2) for subsequent use by mixing in dry for step (1) 60 ~ 90 parts of semi-aromatic nylon resins, 10-25 part inorganic mineral filler and 5 ~ 10 parts of compatilizers, 0.5 ~ 2 part of oxidation inhibitor, 0.3 ~ 1 part of coupling agent, 1 ~ 3 part of lubricant high-speed mixer;
(3) add from main spout the raw material mixed step (2);
(4) then remaining 0-15 part inorganic mineral filler is added from side spout, through twin screw extruder tie rod, cooling, pelletizing, drying, packaging.
In described step (1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
Mixing time in described step (2) is 5 ~ 10min;
In described step (4), each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Beneficial effect of the present invention is as follows:
1. through the semi-aromatic nylon that inorganic mineral is filling-modified, can significantly improve its intensity, rigidity, mineral-filled semi-aromatic nylon has good apparent mass in addition, and processing characteristics is flowing with great difficulty, the shaping advantage such as soon.
2. inorganic mineral filler used, by silane coupling agent process, makes the binding ability between mineral filler and semi-aromatic nylon resin matrix increase substantially, and ensure that inorganic mineral filler can distribute uniformly in resin matrix.
3. in the course of processing, inorganic mineral filler adds respectively by main spout and side spout, can solve high powder blanking uneven problem when filling content, improve powder degree of scatter, make it be uniformly distributed in matrix resin, ensure the stable of the performance of material.
Embodiment
In order to further illustrate essence of the present invention, now describe the present invention in conjunction with specific embodiments:
Embodiment 1
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, wollastonite 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral fillers and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral fillers are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 2
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, kaolin 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 15 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 15 parts of inorganic mineral filler kaolin are added through melt extruding from side spout, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 3
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T60 part, wollastonite 40 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler wollastonite respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 60 parts, 25 parts of inorganic mineral filler wollastonites and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 15 parts of inorganic mineral fillers are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.Embodiment 4
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T60 part, kaolin 40 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 60 parts, 25 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 15 parts of inorganic mineral filler kaolin are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 5
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA9T70 part, wollastonite 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler wollastonites and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler wollastonites are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 6
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA9T70 part, kaolin 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler kaolin are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 7
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA12T70 part, wollastonite 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler wollastonites and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler wollastonites are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 8
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA12T70 part, kaolin 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler kaolin are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 9
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, wollastonite 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of positive titanium isopropylate, Zinic stearas 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler wollastonites and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler wollastonites are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 10
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, kaolin 30 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of positive titanium isopropylate, Zinic stearas 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 20 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) then 10 parts of inorganic mineral filler kaolin are added from side spout, through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 11
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, wollastonite 10 parts, maleic anhydride graft vinylbenzene 5 parts, β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester 0.5 part, 0.3 part positive titanium isopropylate, Zinic stearas 1 part;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 10 parts of inorganic mineral filler wollastonites and compatilizer 5 parts, 0.5 part, oxidation inhibitor, coupling agent 0.3 part, lubricant 1 part of input high-speed mixer, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 12
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T70 part, kaolin 10 parts, maleic anhydride graft vinylbenzene 10 parts, β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester 2 parts, 1 part positive titanium isopropylate, Zinic stearas 3 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 10 parts of inorganic mineral filler kaolin and compatilizer 5 parts, 2 parts, oxidation inhibitor, coupling agent 1 part, lubricant 3 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 13
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T90 part, wollastonite 10 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 70 parts, 10 parts of inorganic mineral filler wollastonites and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
Embodiment 14
A kind of inorganic mineral fills semi-aromatic nylon composite, be made up of the raw material of following weight part: semi-aromatic nylon resin PA10T90 part, kaolin 10 parts, maleic anhydride 8 parts, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1.5 parts, 0.7 part of γ-aminopropyl triethoxysilane, calcium stearate 2 parts;
Preparation method:
(1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
(2) by the semi-aromatic nylon resin in step (1) 90 parts, 10 parts of inorganic mineral filler kaolin and compatilizer 8 parts, 1.5 parts, oxidation inhibitor, coupling agent 0.7 part, lubricant 2 parts of input high-speed mixers, Homogeneous phase mixing 5 ~ 10min;
(3) add from main spout the raw material mixed step (2);
(4) through melt extruding, granulation; Each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
The concrete test data of performance that embodiment 1-4 obtains product is as shown in table 1.
Table 1
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.

Claims (10)

1. a semi-aromatic nylon composite, is characterized in that: be made up of the component comprising following weight part:
2. semi-aromatic nylon composite according to claim 1, is characterized in that: described semi-aromatic nylon resin be selected from PA4T, PA6T, PA7T, PA8T, PA9T, PA10T, PA12T, PA13T or PA14T one or more.
3. semi-aromatic nylon composite according to claim 1, is characterized in that: described inorganic mineral filler is one or more in mica, wollastonite, talcum powder, calcium carbonate, barium sulfate or kaolin.
4. semi-aromatic nylon composite according to claim 1, is characterized in that: described compatilizer is one or more of maleic anhydride, maleic anhydride-g-SBS, maleic anhydride graft vinylbenzene or maleic anhydride grafted ethene-octene copolymer.
5. semi-aromatic nylon composite according to claim 1, is characterized in that: described oxidation inhibitor phenols high-temperature antioxidant is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, 1,3,5-tri-(the 4-tertiary butyl-3-hydroxyl-2,6-dimethyl benzyl)-1,3,5-triazine-2,4,6-(1H, 3H, 5H) one or more in-triketone.
6. semi-aromatic nylon composite according to claim 1, is characterized in that: described coupling agent is the one or more than one in vinyltriethoxysilane, γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, γ-propyl methacrylate base silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, positive titanium isopropylate or the different stearoyl titanic acid ester of sec.-propyl three.
7. semi-aromatic nylon composite according to claim 1, is characterized in that: described lubricant is calcium stearate or Zinic stearas.
8. the preparation method of arbitrary described semi-aromatic nylon composite in claim 1-7, is characterized in that: comprise the following steps:
(1) first semi-aromatic nylon, inorganic mineral filler are put into respectively loft drier forced air drying for subsequent use;
(2) for subsequent use by mixing in 60 ~ 90 parts of dry for step (1) semi-aromatic nylon resins, 10-25 part inorganic mineral filler, 5 ~ 10 parts of compatilizers, 0.5 ~ 2 part of oxidation inhibitor, 0.3 ~ 1 part of coupling agent, 1 ~ 3 part of lubricant high-speed mixer;
(3) add from main spout the raw material mixed step (2);
(4) then 0-15 part inorganic mineral filler is added from side spout, through twin screw extruder tie rod, cooling, pelletizing, drying, packaging.
9. method according to claim 1, is characterized in that: in described step (1) by semi-aromatic nylon resin, inorganic mineral filler respectively at 100 ~ 120 DEG C and 110 ~ 130 DEG C of forced air dryings 6 ~ 8 hours;
Mixing time in described step (2) is 5 ~ 10min.
10. method according to claim 1, it is characterized in that: in described step (4), each section of temperature of twin screw extruder is set as: district's temperature 275 ± 10 DEG C, two district's temperature 275 ± 10 DEG C, three district's temperature 280 ± 10 DEG C, four district's temperature 285 ± 10 DEG C, five district's temperature 295 ± 10 DEG C, six district's temperature 295 ± 10 DEG C, seven district's temperature 295 ± 10 DEG C, eight district's temperature 290 ± 10 DEG C, nine district's temperature 285 ± 10 DEG C, ten district's temperature 285 ± 10 DEG C, head temperature is 285 ± 10 DEG C, screw speed 250 ~ 350 revs/min.
CN201310368483.6A 2013-08-21 2013-08-21 Inorganic mineral filled semi-aromatic nylon composite material and preparation method thereof Pending CN104419195A (en)

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CN106928702A (en) * 2015-12-31 2017-07-07 上海杰事杰新材料(集团)股份有限公司 A kind of high temperature resistant nylon/polyphenylene oxide composite material and preparation method thereof
CN109097854A (en) * 2018-08-14 2018-12-28 安徽和邦纺织科技有限公司 A kind of preparation method by polyamide modified polyester fiber
CN111004497A (en) * 2019-12-24 2020-04-14 上海中镭新材料科技有限公司 Electroplating nylon material and preparation method thereof

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CN101885914A (en) * 2010-07-13 2010-11-17 东莞市意普万工程塑料有限公司 Composite material special for automobile engine oil pan and preparation method thereof
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CN106566233A (en) * 2015-10-13 2017-04-19 上海杰事杰新材料(集团)股份有限公司 Nano-talcum powder toughened and strengthened high-temperature-resistant nylon composite material and preparation method thereof
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CN111004497A (en) * 2019-12-24 2020-04-14 上海中镭新材料科技有限公司 Electroplating nylon material and preparation method thereof
CN111004497B (en) * 2019-12-24 2022-03-29 上海中镭新材料科技有限公司 Electroplating nylon material and preparation method thereof

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Application publication date: 20150318