CN106280435A - A kind of heat resistant PA material and preparation method thereof - Google Patents

A kind of heat resistant PA material and preparation method thereof Download PDF

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Publication number
CN106280435A
CN106280435A CN201610793519.9A CN201610793519A CN106280435A CN 106280435 A CN106280435 A CN 106280435A CN 201610793519 A CN201610793519 A CN 201610793519A CN 106280435 A CN106280435 A CN 106280435A
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CN
China
Prior art keywords
heat resistant
preparation
lubricant
age resister
glass
Prior art date
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Pending
Application number
CN201610793519.9A
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Chinese (zh)
Inventor
张钊鹏
姚大爱
肖雄伟
张平
陈东明
杨子江
林嗣鑫
郑梓灿
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Guangdong Shunde Shunyan New Material Co Ltd
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Guangdong Shunde Shunyan New Material Co Ltd
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Priority to CN201610793519.9A priority Critical patent/CN106280435A/en
Publication of CN106280435A publication Critical patent/CN106280435A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

Abstract

The invention discloses a kind of heat resistant PA material and preparation method thereof.Described heat resistant PA material is to be prepared from by 60 calculated by weight percentage~the PA6 of the PA66 of 70%, 5~10%, age resister 0.5~1%, lubricant 0.4~1%, glass 20~30%.The present invention is by compounding with polynary age resister, it is achieved long-term heat resistant effect so that goods can be with life-time service under 160 DEG C of environment, and the heat resistant time was more than 3000 hours.

Description

A kind of heat resistant PA material and preparation method thereof
Technical field
The invention belongs to macromolecular material and processing technique field thereof, be specifically related to a kind of heat resistant PA material and Preparation method.
Background technology
Polyamide (Polyamide, PA) is a kind of widely used engineering plastics, its molecular structure and crystallization, Make it have excellent physics, machine performance.Yet with the existence of amide polar group, the water absorption rate of polyamide is high, thermal deformation Temperature is low, and modulus and intensity are the highest, limits its application.Polyamide 66, English name Polyamide 66 (being called for short PA66), It is the general name of the high polymer in macromolecular main chain repetitive containing amide group.Be in five large-engineering plastics yield maximum, The kind that kind is at most, purposes is the widest.It is widely used in and manufactures machinery, automobile, chemistry and the part of electric device, such as gear, rolling Impeller in son, pulley, roll shaft, the pump housing, fan blade, high pressure sealing enclose, valve seat, pad, lining, various handle, bracing frame, electricity Line bag internal layer etc..
Normally, owing to heat produced when electromotor works is through overshoot, conduction, convection current and by atmospheric environment shadow Ringing, the temperature range in hood is-40 DEG C~160 DEG C.Particularly stopping after running car at that moment, it is the highest Temperature to reach about 160 DEG C.Therefore the heat-resisting of material to its periphery is very important, examines from life-time service and birthday noodle Consider, the heat-resisting of material of its periphery must be reached 160 DEG C, and industry to its determined standard be resistance to 160 DEG C 3000 hours, Mechanical property decay is less than 30%.Although PA material high-temperature resistant result is good, but also it is the effect of short-term, for up to 2000 More than hour, conventional PA material does not still reach ideal effect.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of heat resistant PA material, pass through Compound with polynary age resister, it is achieved long-term heat resistant effect so that goods under 160 DEG C of environment can with life-time service, The heat resistant time was more than 3000 hours.
For solving the problems referred to above, the technical solution adopted in the present invention is as follows:
A kind of heat resistant PA material, it is to be prepared from by the following raw material calculated by weight percentage:
PA66 60~70%
PA6 5~10%
Age resister 0.5~1%
Lubricant 0.4~1%
Glass 20~30%
Wherein, the percetage by weight sum of raw material is 100%.
As further scheme, heat resistant PA material of the present invention be by calculate by weight percentage with Lower raw material is prepared from:
PA66 63.6%
PA6 5%
Age resister 0.8%
Lubricant 0.6%
Glass 30%.
In heat resistant PA material of the present invention, as further scheme, described PA66 is that viscosity is at 2.6- 3.0Pa·s。
In heat resistant PA material of the present invention, as further scheme, described PA6 is that viscosity is at 2.6- 3.0Pa·s。
In heat resistant PA material of the present invention, as further scheme, described age resister is double (2.4- Di-tert-butyl-phenyl) pentaerythritol diphosphites and the mixture of mantoquita.
In heat resistant PA material of the present invention, as further scheme, described lubricant is calcium stearate Or zinc stearate.
Another object of the present invention is to provide the preparation method of a kind of heat resistant PA material, by this preparation method Obtain a kind of heat resistant PA material, significantly improve the heat resistant effect of PA material;Concrete scheme is as follows:
A kind of preparation method of heat resistant PA material, this preparation method comprises the following steps:
1) first with high mixer, PA66 and PA6 is stirred, and eliminate the moisture on surface, obtain mixture polyamides Amine;
2) then age resister and lubricant first being premixed and add in said mixture polyamide afterwards, stirring is all Even, obtain premix material;
3) above-mentioned premix material is proceeded to melt extrude in double screw extruder pelletize.
In heat resistant PA material preparation method of the present invention, as further scheme, step 1) stirring time Between be 3-8 minute, rotating speed is 1000-1500r/min.
In heat resistant PA material preparation method of the present invention, as further scheme, step 2) aging resistance The time that agent and lubricant are mixed is 5~8min.
In heat resistant PA material preparation method of the present invention, as further scheme, step 3) in, extrusion Temperature is 230-275 DEG C, and the rotating speed of twin screw is 100-150r/min.
Compared to existing technology, the beneficial effects of the present invention is:
Heat resistant PA material the most of the present invention is compounding by PA66 Yu PA6, and combines glass and make inorganic filler, The heat resistant effect of PA material can be significantly improved, it is achieved long-term heat resistant effect so that goods are at 160 DEG C of environment Under can be with life-time service, the heat resistant time was more than 3000 hours;
In the preparation method of heat resistant PA material the most of the present invention, first by two kinds of polyamide raw materials high mixers By the moisture removal on raw material surface, be conducive to improving the stability of PA materials processing performance;
In the preparation method of heat resistant PA material the most of the present invention, by first that age resister is equal with lubricant Premix with mixed polyamide again after Hun, be beneficial to the dispersion with PA resin, it is ensured that the homogeneity of heat resistant PA material is with stable Property.
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Detailed description of the invention
Heat resistant PA material of the present invention, it is by the following raw material preparation calculated by weight percentage Become:
PA66 60~70%
PA6 5~10%
Age resister 0.5~1%
Lubricant 0.4~1%
Glass 20~30%
Wherein, the percetage by weight sum of raw material is 100%.
As further scheme, heat resistant PA material of the present invention be by calculate by weight percentage with Lower raw material is prepared from:
PA66 63.6%
PA6 5%
Age resister 0.8%
Lubricant 0.6%
Glass 30%.
" PA66 refers to " polyamide 66 mentioned in the present invention, namely nylon66 fiber.Owing to PA66 water absorption is relatively big, size Less stable, and intensity is not as good as metallic aluminium, limits its application in some structural material;The mechanical property master of PA 66 Depend on chemical bond and the intermolecular force of its molecular backbone.The fracture of chemical bond and intermolecular force on molecular backbone Interference all will result directly in the transformation of nylon high polymer bulk properties.Strengthen the polarity of molecule or increase intermolecular hydrogen bonding all Help the intensity improving material.But polar group too much can hinder the activeness of main chain, thus reduces the toughness of nylon so that it is Fragility rises.After adding certain filler, the water absorption rate of PA declines, and dimensional stability improves, and intensity is by filling intensity and affine Degree affects and raises accordingly.Owing to inorganic filler can improve the crystallinity of polymeric matrix material to a great extent Energy, heat decomposition temperature, heat distortion temperature, mechanical strength, antiwear and antifriction, the purpose such as fire-retardant, corrosion-resistant, and then reach to improve polymerization The purpose of the combination property of thing matrix material.Because of glass i.e. glass fibre there is good insulating, thermostability is strong, corrosion resistance good, Mechanical strength advantages of higher, the filler in PA66 material can be effectively improved the performance of PA66, in the present invention, it is preferred to Use roving glass fiber as inorganic filler;Because roving glass fiber is to be interleaved with each other lack of alignment together in the composite, and not Streamwise arrangement in the composite as short glass fiber.Compared with short glass fiber composite, the most this lack of alignment State and the increase of Length of Glass Fiber, make roving glass fiber composite material exhibits go out higher mechanical property, the thermostability of excellence, endurance Property and wearability, and preferably fillibility, low warpage properties and isotropism etc..Owing to long stapled fibrous termination is less, phase Having contributed in performance than short glass fiber composite.Further, since the fusing point that the fusing point of PA6 is far below PA66, have Wider processes temperature, therefore, can reduce the temperature of the equipment adding man-hour in the present invention by adding PA6.
Studying discovery in the present invention, the mechanical property of PA66 improves with the increase of content of glass fiber, but works as content After 50%, performance increase is obstructed;Simultaneously because content of glass fiber increases, processing fluidity can be made to decline, moulding process It is deteriorated.Content of glass fiber increases, and the arbitrary cross section of composite just has greater number of glass to carry, the extraction of these glasses Or fracture, need to apply bigger load, thus improve hot strength and the bending strength of composite.Simultaneously as glass The increase of fine volume content, i.e. resin bed between glass and glass is thinning, and effect stress on the composite is easy to pass through Resin bed and in glass transmit, the deformation of resin is also retrained by glass, thus the modulus of elasticity in static bending is also with glass fiber content Increase and improve.Therefore considering, in above-mentioned formula, the consumption of glass is 20-30%.
Owing to the viscosity of PA66 is very sensitive for variations in temperature, go and viscosity has certain shadow to the shrinkage factor of PA66 Ring.Therefore, the PA material moderate in order to obtain shrinkage factor, in heat resistant PA material of the present invention, as entering one The scheme of step, described PA66 is that viscosity is at 2.6-3.0Pa s.
In heat resistant PA material of the present invention, as further scheme, described PA6 is that viscosity is at 2.6- 3.0Pa·s。
In heat resistant PA material of the present invention, as further scheme, described age resister is double (2.4- Di-tert-butyl-phenyl) pentaerythritol diphosphites (antioxidant 627A) and the mixture of mantoquita.Cu in copper salt antioxidantn+ Stable complex structure can be formed with the atom N on polyamide molecule amide groups, play oxygen on stable polyamides strand The effect of atom.Additionally, the hydroperoxide decomposition that polyamide generates during thermal-oxidative ageing can be non-by mantoquita Free radical product, thus the carrying out of inhibitory activity free radical chain aging reaction, it is to avoid macromolecule chain break, decomposing hydrogen mistake Cu during oxiden+Act primarily as catalytic action, itself consume few, so in the present invention by antioxidant and mantoquita Compounding, the thermo oxidative aging efficiency in PA resin is the highest.
In heat resistant PA material of the present invention, as further scheme, described lubricant is calcium stearate Or zinc stearate.
Another object of the present invention is to provide the preparation method of a kind of heat resistant PA material, by this preparation method Obtain a kind of heat resistant PA material, significantly improve the heat resistant effect of PA material;Concrete scheme is as follows:
A kind of preparation method of heat resistant PA material, this preparation method comprises the following steps:
1) first with high mixer, PA66 and PA6 is stirred, and eliminate the moisture on surface, obtain mixture polyamides Amine;
2) then age resister and lubricant first being premixed and add in said mixture polyamide afterwards, stirring is all Even, obtain premix material;
3) above-mentioned premix material is proceeded to melt extrude in double screw extruder pelletize.
In heat resistant PA material preparation method of the present invention, as further scheme, step 1) stirring time Between be 3-8 minute, rotating speed is 1000-1500r/min.
In heat resistant PA material preparation method of the present invention, as further scheme, step 2) aging resistance The time that agent and lubricant are mixed is 5~8min.
The research of the present invention finds, improves screw speed and increase the active force between glass and resin, it is easier to Causing the fracture of glass, Length of Glass Fiber reduces accordingly, and mechanical property can decline accordingly.Heat resistant the most of the present invention In PA material preparation method, as further scheme, step 3) in, extrusion temperature is 230-275 DEG C, and the rotating speed of twin screw is 100-150r/min。
The following is some embodiments of the present invention, in the following embodiments, at raw material, reagent and the equipment used Outside particular determination, all can be obtained by commercial channel.
Embodiment 1
A kind of heat resistant PA material, its percentage includes following components:
PA66 63.6%
PA6 5%
Age resister 0.8%
Lubricant 0.6%
Glass 30%;
1) first with high mixer, PA66 and PA6 is stirred 3 minutes with the rotating speed of 1500r/min, and eliminate the water on surface Point, obtain mixture polyamide;
2) then first carry out premixing 5 minutes by age resister and lubricant, be then added in said mixture polyamide, continue Continuous stirring 10 minutes, obtains premix material;
3) above-mentioned premix material proceeding to melt extrude in double screw extruder pelletize, wherein extrusion temperature is 230 DEG C, double spiral shells The rotating speed of bar is 150r/min.
Embodiment 2
A kind of heat resistant PA material, its percentage includes following components:
PA66 63.2%
PA6 5%
Age resister 1%
Lubricant 0.8%
Glass 30%;
The preparation method of above-mentioned heat resistant PA material is:
1) first with high mixer, PA66 and PA6 is stirred 5 minutes with the rotating speed of 1200r/min, and eliminate the water on surface Point, obtain mixture polyamide;
2) then first carry out premixing 6 minutes by age resister and lubricant, be then added in said mixture polyamide, continue Continuous stirring 12 minutes, obtains premix material;
3) above-mentioned premix material proceeding to melt extrude in double screw extruder pelletize, wherein extrusion temperature is 255 DEG C, double spiral shells The rotating speed of bar is 120r/min.
Embodiment 3
A kind of heat resistant PA material, its percentage includes following components:
PA66 60.2%
PA6 8%
Age resister 1%
Lubricant 0.8%
Glass 30%;
The preparation method of above-mentioned heat resistant PA material is:
1) first with high mixer, PA66 and PA6 is stirred 8 minutes with the rotating speed of 1000r/min, and eliminate the water on surface Point, obtain mixture polyamide;
2) then first carry out premixing 8 minutes by age resister and lubricant, be then added in said mixture polyamide, continue Continuous stirring 15 minutes, obtains premix material;
3) above-mentioned premix material proceeding to melt extrude in double screw extruder pelletize, wherein extrusion temperature is 275 DEG C, double spiral shells The rotating speed of bar is 100r/min.
Performance test
Heat resistant PA material obtained by above-described embodiment 1-3 is carried out Mechanics Performance Testing, Mechanics Performance Testing Environment: 23 DEG C, dry state, test event, the standard of test institute foundation and the results are shown in Table 1.
Table 1: mechanical experimental results
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to limit the scope of protection of the invention with this, The change of any unsubstantiality that those skilled in the art is done on the basis of the present invention and replacement belong to institute of the present invention Claimed scope.

Claims (10)

1. a heat resistant PA material, it is characterised in that it is by the following raw material preparation calculated by weight percentage Become:
PA66 60~70%
PA6 5~10%
Age resister 0.5~1%
Lubricant 0.4~1%
Glass 20~30%
Wherein, the percetage by weight sum of raw material is 100%.
Heat resistant PA material the most according to claim 1, it is characterised in that it is by calculating by weight percentage Following raw material is prepared from:
PA66 63.6%
PA6 5%
Age resister 0.8%
Lubricant 0.6%
Glass 30%.
Heat resistant PA material the most according to claim 1 and 2, it is characterised in that described PA66 is that viscosity is at 2.6- 3.0Pa·s。
Heat resistant PA material the most according to claim 1 and 2, it is characterised in that described PA6 is that viscosity is at 2.6- 3.0Pa·s。
Heat resistant PA material the most according to claim 1 and 2, it is characterised in that described age resister is double (2.4- Di-tert-butyl-phenyl) pentaerythritol diphosphites and the mixture of mantoquita.
Heat resistant PA material the most according to claim 1 and 2, it is characterised in that described lubricant is calcium stearate Or zinc stearate.
7. the preparation method of a heat resistant PA material as claimed in claim 1 or 2, it is characterised in that this preparation side Method comprises the following steps:
1) first with high mixer, PA66 and PA6 is stirred, and eliminate the moisture on surface, obtain mixture polyamide;
2) then age resister and lubricant are first premixed and add afterwards in said mixture polyamide, stir, To premix material;
3) above-mentioned premix material is proceeded to melt extrude in double screw extruder pelletize.
Preparation method the most according to claim 7, it is characterised in that step 1) mixing time is 3-8 minute, rotating speed is 1000-1500r/min。
Preparation method the most according to claim 7, it is characterised in that step 2) time of being mixed with lubricant of age resister It is 5~8min.
Preparation method the most according to claim 7, it is characterised in that step 3) in, extrusion temperature is 230-275 DEG C, double The rotating speed of screw rod is 100-150r/min.
CN201610793519.9A 2016-08-31 2016-08-31 A kind of heat resistant PA material and preparation method thereof Pending CN106280435A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108915912A (en) * 2018-07-11 2018-11-30 江阴市农业药械厂 Heat-insulated and heat-resisting air inlet pipe pad and its manufacturing method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5872175A (en) * 1997-07-08 1999-02-16 Hyundai Mortor Company Polyamide resin composition
CN101760016A (en) * 2008-11-21 2010-06-30 上海普利特复合材料股份有限公司 Flame-retarded enhanced PA66 composite special for wire connector box
CN104004348A (en) * 2014-06-06 2014-08-27 宁波伊德尔新材料有限公司 High-thermal-oxidative stability and heat-resistant regeneration nylon material and preparation method thereof
CN105111730A (en) * 2015-04-16 2015-12-02 宁波伊德尔新材料有限公司 Glass fiber reinforced nylon 66 composite material for panel of dish-washing machine and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5872175A (en) * 1997-07-08 1999-02-16 Hyundai Mortor Company Polyamide resin composition
CN101760016A (en) * 2008-11-21 2010-06-30 上海普利特复合材料股份有限公司 Flame-retarded enhanced PA66 composite special for wire connector box
CN104004348A (en) * 2014-06-06 2014-08-27 宁波伊德尔新材料有限公司 High-thermal-oxidative stability and heat-resistant regeneration nylon material and preparation method thereof
CN105111730A (en) * 2015-04-16 2015-12-02 宁波伊德尔新材料有限公司 Glass fiber reinforced nylon 66 composite material for panel of dish-washing machine and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108915912A (en) * 2018-07-11 2018-11-30 江阴市农业药械厂 Heat-insulated and heat-resisting air inlet pipe pad and its manufacturing method

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