CN109705568A - A kind of low precipitation fire-retardant polyamide material of low smell, preparation method and application - Google Patents
A kind of low precipitation fire-retardant polyamide material of low smell, preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of low precipitation fire-retardant polyamide material of low smell, preparation method and application, the low precipitation fire-retardant polyamide material of the low smell, is grouped as: polyamide 84.5%~92%, fire retardant 7%~13%, eliminating smell agent 0.5%~1.5%, lubricant 0.3%~0.5%, antioxidant 0.2%~0.5% by the group of following weight percent meter；Wherein, fire retardant is melamine cyanurate flame retardant；Eliminating smell agent is the composition of organic zinc salt and Si-Al molecular sieve；Organic zinc salt is can response type Long carbon chain organic zinc salt；Partial size≤15 μm of Si-Al molecular sieve.The low precipitation fire-retardant polyamide material of low smell provided by the invention not only has good flame retardant property, but also there is lower fire retardant small molecule to be precipitated, less injection mold deposition problems and product odour problem.The low precipitation fire-retardant polyamide material of the low smell can be suitable for the demanding automotive electronics electric field of material oder levels.
Description
Technical field
The present invention relates to MCA fire-retardant polyamide material, in particular to the low precipitation fire-retardant polyamide material of a kind of low smell, its
Preparation method and application.
Background technique
Polyamide (nylon, PA) is that yield is big, one of wide in variety and five large-engineering plastics wide purposes.Nylon has very high
Mechanical strength, high softening-point, heat resistance, wear resistance, oil resistivity, weak acid resistant, alkaline-resisting, resistance to general organic solvent, electricity absolutely
Edge and have self-extinguishment.Nylon material is respectively led in automobile industry, electric industry, communications and transportation, machinery, aerospace etc.
Domain is all widely used.Wherein, fire-retardant nylon material electrically waits the application requirement in fields fire-retardant, environmentally friendly and strong in automotive electronics
Health.
With the continuous improvement of environmental requirement, traditional bromide fire retardant has been unable to meet European Union RoHS and WEEE instruction
It is required that and environmentally friendly bromide fire retardant also due to exhaust gas volumn is big when burning, generate the problems such as corrosive gas more and more attention has been paid to.
Red phosphorus combustion inhibitor also limits it in fire-retardant nylon due to the problems such as self color problem, hydrogen phosphide harm, metal protection
Application.From the point of view of current industry development trend, fire-retardant nylon material is non-halogen to meet environmentally protective development trend, and electricity
A kind of development trend requirement of the industries such as sub electrical to fire-retardant nylon material.In automotive electronics electric material application field, such as answer
Used in fields such as automotive connector, connector and connecting terminals, more and more clients not only want the flame retardant rating of material
It asks, while also having the smell control of material compared with strict requirements.
Melamine cyanurate (MCA) halogen-free flame retardants is good due to having in non-reinforcing halogen-free flame-retardant PA 66/PA6
Flame retardant property, burn the raw few and high relative discharge tracking index CTI of smoke, which is widely used in connector, connector
With the fields such as connecting terminal.But it is analyzed for existing MCA fire-retardant nylon technology of preparing, prepares material and squeezing out and be molded
Cheng Zhong, the problems such as being also easy to produce precipitation and mold deposits.There is disclosure melamine class in DSM N. V. in patent US2001008913A1
Fire retardant is easy to block vacuum in process and generates small molecule mold deposits in injection moulding process, and MCA is being higher than
Generation micro-molecular gas is decomposed in aggravation under 270 DEG C of processing temperatures causes product injection molding unstable.TORAY company is in patent
There is detailed analysis melamine class fire-retardant nylon material in extrusion or injection moulding process in US4383064A patent, melamine
Small molecule is easy literization and is deposited on mold or surface of shaped parts.
These existing patents essentially describe MCA fire-retardant nylon and squeeze out in product or the problem of injection moulding process and fire retardant
Precipitation problem is decomposed, however there is no further disclose because MCA fire-retardant nylon material is in extruding pelletization process, injection molding front baking for patent
During material process, product injection moulding process or shaped article are delivered for use, it can all give out bigger ammonia taste and engender a repugnance sense,
It will lead to biggish smell problem in automotive electronics electrical applications.
Summary of the invention
Bigger ammonia taste can be given out in order to solve to mention MCA fire-retardant nylon material in background technique to engender a repugnance
Sense, the present invention provide a kind of low smell low precipitation fire-retardant polyamide material, are grouped as by the group of following weight percent meter:
Polyamide: 84.5%~92%；
Fire retardant: 7%~13%；
Eliminating smell agent: 0.5%~1.5%；
Lubricant: 0.3%~0.5%；
Antioxidant: 0.2%~0.5%；
Wherein, the fire retardant is melamine cyanurate (MCA) fire retardant；
The eliminating smell agent is the composition of organic zinc salt and Si-Al molecular sieve；Organic zinc salt be can response type Long carbon chain have
Machine zinc salt；Si-Al molecular sieve has porous structure；Partial size D99≤15 μm of Si-Al molecular sieve.
Further, the polyamide includes nylon66 fiber (PA66) resin slicer and nylon 6 (PA6) toner；Nylon
66 resin slicer relative viscosities (R.V.) are 2.4~2.8；Nylon 6 resin powder relative viscosity is 2.4~2.8；Nylon 66 resin
Slice and nylon 6 resin powder weight ratio are 7~10:0.5~1；Nylon 6 resin powder is the powder of 80~200 mesh partial sizes
Resin.
Further, partial size D99≤50 μm of the melamine cyanurate flame retardant.
Further, the lubricant is one of stearate, ethylene acrylic acid co polymer and amide series lubricant agent
Or it is several.
Further, the antioxidant is one of Hinered phenols primary antioxidant, phosphorous acid esters auxiliary anti-oxidant or several
Kind.
The present invention also provides a kind of low preparation methods that fire-retardant polyamide material is precipitated of low smell, comprising the following steps:
Step 1 puts into first part's polyamide and fire retardant in high-speed mixer, is uniformly mixed, and fire retardant is made
Powder packet, it is spare；
Step 2 puts into eliminating smell agent, lubricant and antioxidant in low-speed mixer, is uniformly mixed, and auxiliary agent packet is made,
It is spare；
Step 3 throws auxiliary agent packet made from second part polyamide and step 2 from the main spout of double screw extruder
Material；Fire retardant powder packet made from step 1 is individually fed intake from the side spout of double screw extruder；It squeezes out, crosses water cooling, cut
The low precipitation fire-retardant polyamide material of low smell is made after grain.
Further, the double screw extruder in step 3 has black soy sauce vacuum function.
Further, first part's polyamide in step 1 is nylon 6 resin powder；The middle second part polyamides of step 3
Amine is nylon 66 resin slice.
The present invention also provides a kind of low application that fire-retardant polyamide material is precipitated of low smell, the low smell is low be precipitated it is fire-retardant
Polyamide material is used as automotive electronics electrical equipment material.
Compared with prior art, the beneficial effects of the present invention are:
(1) of the invention use can response type Long carbon chain organic zinc salt compounding Si-Al molecular sieve (partial size D99≤15 μm) work
For eliminating smell agent, there is the fire-retardant polyamide material prepared lower fire retardant small molecule to be precipitated, less injection mold deposits
Problem and lower smell, and compounding eliminating smell agent does not influence the flame retardant property and toughness of material of material.
(2) fire-retardant compared to directly being prepared by the way of the one pot of blanking of main spout using the double screw extruder singly vacuumized
Polyamide material, the invention patent uses the double screw extruder with black soy sauce vacuum and MCA fire retardant and PA6 toner are pre-
It is fed after mixed by side spout.The small molecule precipitation ingredient generated in production process is few, and the small molecule being precipitated can be double
It is come out at the double vacuum ports of screw extruder by more effective devolatilization, the smell of product can be reduced.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
It should be noted that the examples of the embodiments are intended to be used to explain the present invention, and should not be understood as to the present invention
Limitation, in the examples where no specific technique or condition is specified, according to the literature in the art described technology or conditions or
Person carries out according to product description, reagents or instruments used without specified manufacturer, and being can be by the normal of commercially available acquisition
Advise product.
Wherein, it should be noted that it is of the invention can response type Long carbon chain organic zinc salt refer to ricinoleic acid zinc salt, preferably
Win wound EVONIK odour absorbentsSorb PY 88 TQ.Si-Al molecular sieve refers to SiO2/Al2O3=220~400 (rub
That ratio) high silica alumina ratio ZSM-5 molecular sieve.Double screw extruder with black soy sauce vacuum function refers to that draw ratio is the Rhea of 40:1
The double screw extruder of the bis- vacuum models of RXT-65.
The present invention provides embodiment 1-4 as shown in Table 1 and comparative example 1-4 each group distribution ratio (by weight percentage):
Table 1
Wherein, eliminating smell agent by can response type Long carbon chain organic zinc salt and Si-Al molecular sieve mixing form, can response type it is long
The weight ratio of carbochain organic zinc salt and Si-Al molecular sieve is 5:95.
The preparation method of embodiment 1-4:
Step 1 weighs PA6 toner and MCA fire retardant by the proportion of table 1, and puts into high-speed mixer, revolving speed
600r/min mixes 2min, is sufficiently mixed and is formed uniformly fire retardant powder packet, spare；
Step 2 is weighed eliminating smell agent, calcium stearate and antioxidant 1098 by the proportion of table 1, and puts into low-speed mixer
In, revolving speed 100r/min mixes 5min, is sufficiently mixed and is formed uniformly auxiliary agent packet, spare；
Step 3 weighs PA66 resin slicer by the proportion of table 1, and the auxiliary agent packet that PA66 resin slicer and step 2 are obtained is distinguished
Claim to feed from the main spout weightlessness blanking of double screw extruder by weightlessness；The fire retardant powder packet that step 1 is obtained is independent
Pass through the weightless side spout metering feeding claimed from double screw extruder；Twin-screw extrusion vacuum number is double vacuum, vacuum degree-
0.09MPa；The temperature of each section of double screw extruder is respectively as follows: 220 DEG C, and 255 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 255 DEG C, 245
DEG C, 245 DEG C, 245 DEG C, 260 DEG C, head temperature is 270 DEG C, screw speed 400r/min；Shearing, mixing of the material in screw rod
With the lower sufficiently fusion of conveying, finally by extrusion, tie rod, cross that water is cooling, low smell is made after pelletizing low precipitation Flameproof polyamide
Finished pellets.
The preparation method of comparative example 1:
Step 1 weighs PA66 resin slicer, PA6 resin slicer, MCA fire retardant, eliminating smell agent, antioxidant by the proportion of table 1
1098 and calcium stearate, and weighed whole materials are added in high-speed mixer together, revolving speed 600r/min mixes 2min,
It is sufficiently mixed to obtain mixed material, it is spare；
Step 2, the mixed material for obtaining step 1 pass through the weightless main spout weightlessness blanking claimed from double screw extruder
Charging；Twin-screw extrusion vacuum number is double vacuum, vacuum degree -0.09MPa；The temperature of each section of double screw extruder is respectively as follows: 220
DEG C, 255 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 255 DEG C, 245 DEG C, 245 DEG C, 245 DEG C, 260 DEG C, head temperature is 270 DEG C, screw rod
Revolving speed is 400r/min；Material sufficiently fuses under the shearing, mixing and conveying of screw rod, finally passes through extrusion, tie rod, crosses water cooling
But, Flameproof polyamide finished pellets are made after pelletizing.
The preparation method of comparative example 2:
Step 1 weighs PA66 resin slicer, PA6 resin slicer, eliminating smell agent, calcium stearate and antioxidant by the proportion of table 1
1098, and weighed material is added in high-speed mixer together, revolving speed 600r/min, 2min is mixed, is sufficiently mixed and is mixed
Material is closed, it is spare；
Step 2, the mixed material for obtaining step 1 pass through the weightless main spout weightlessness blanking claimed from double screw extruder
Charging；MCA fire retardant is weighed by the proportion of table 1, and separately through the weightless side spout metering feeding claimed from double screw extruder；
Twin-screw extrusion vacuum number is double vacuum, vacuum degree -0.09MPa；The temperature of each section of double screw extruder is respectively as follows: 220 DEG C,
255 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 255 DEG C, 245 DEG C, 245 DEG C, 245 DEG C, 260 DEG C, head temperature is 270 DEG C, and screw rod turns
Speed is 400r/min；Material sufficiently fuses under the shearing, mixing and conveying of screw rod, finally passes through extrusion, tie rod, crosses water cooling
But, Flameproof polyamide finished pellets are made after pelletizing.
The preparation method of comparative example 3:
Step 1 weighs PA6 toner and MCA fire retardant by the proportion of table 1, and is added in high-speed mixer, revolving speed
600r/min mixes 2min, is thoroughly mixed to form fire retardant powder packet, spare；
Step 2 weighs eliminating smell agent, calcium stearate and antioxidant 1098 by the proportion of table 1, and is added in low-speed mixer,
Revolving speed 100r/min mixes 5min, is sufficiently mixed and is formed uniformly auxiliary agent packet, spare；
Step 3 weighs PA66 resin slicer by the proportion of table 1, and the auxiliary agent packet that PA66 resin slicer and step 2 are obtained is distinguished
Claim to feed from the main spout weightlessness blanking of double screw extruder by weightlessness；The fire retardant powder packet that step 1 is obtained is independent
Pass through the weightless side spout metering feeding claimed from double screw extruder；Twin-screw extrusion vacuum number is double vacuum, vacuum degree-
0.09MPa；The temperature of each section of double screw extruder is respectively as follows: 220 DEG C, and 255 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 255 DEG C, 245
DEG C, 245 DEG C, 245 DEG C, 260 DEG C, head temperature is 270 DEG C, screw speed 400r/min；Shearing, mixing of the material in screw rod
With the lower sufficiently fusion of conveying, finally by extrusion, tie rod, cross that water is cooling, Flameproof polyamide finished pellets are made after pelletizing.
The preparation method of comparative example 4:
Step 1 weighs PA6 toner and MCA fire retardant by the proportion of table 1, and puts into high-speed mixer, revolving speed
600r/min mixes 2min, is thoroughly mixed to form fire retardant powder packet, spare；
Step 2 weighs eliminating smell agent, calcium stearate and antioxidant 1098 by the proportion of table 1, and is added in low-speed mixer,
Revolving speed 100r/min mixes 5min, is sufficiently mixed and is formed uniformly auxiliary agent packet, spare；
Step 3 weighs PA66 resin slicer by the proportion of table 1, and the auxiliary agent packet that PA66 resin slicer and step 2 are obtained is distinguished
Claim to feed from the main spout weightlessness blanking of double screw extruder by weightlessness；The fire retardant powder packet that step 1 is obtained is independent
Pass through the weightless side spout metering feeding claimed from double screw extruder；Twin-screw extrusion vacuum number is double vacuum, vacuum degree-
0.09MPa；The temperature of each section of double screw extruder is respectively as follows: 220 DEG C, and 255 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 255 DEG C, 245
DEG C, 245 DEG C, 245 DEG C, 260 DEG C, head temperature is 270 DEG C, screw speed 400r/min；Shearing, mixing of the material in screw rod
With the lower sufficiently fusion of conveying, finally by extrusion, tie rod, cross that water is cooling, Flameproof polyamide finished pellets are made after pelletizing.
By the Flameproof polyamide finished pellets of above-mentioned Experimental comparison example 1-4 and embodiment 1-4 preparation, 90 DEG C of forced air dryings are put
It is dried 4 hours after machine.Then, injection molding obtains test specimens to the particle after drying at a temperature of 255 DEG C~280 DEG C of injection moldings respectively
Item, the correlated performance test of test bars and test method, double screw extruder vacuum condition and fire retardant feeding manner are detailed in
The following table 2 Experimental comparison's table.
Table 2
Remarks :+it is good degree ,+The more the better；It is undesirable level ,-much more bad；
VDA270 standard: (50 ± 5) cm is used3Flameproof polyamide injection molding template is put in closed 1L odor bottle in (80 ± 2)
After toasting 2 hours ± 10min at DEG C.At least 5 people marking, the marking to smell, final we take the average value of several scores, such as
There is decimal, 0.5 is remained larger than to decimal.It is as shown in table 3 to judge scoring criterion:
Table 3
| Ranking score | Standard |
| 1 | Nothing is discovered |
| 2 | Discover, but does not allow people to feel ill |
| 3 | Directly discover, but does not still allow people to feel ill |
| 4 | People is allowed to feel to feel bad |
| 5 | People is allowed to feel to feel bad |
| 6 | It can not receive |
According to table 2, the multinomial performance of embodiment 1-4 is equal it can be seen from comparative example 1-2 and embodiment 1-4 correlation data
Three aspects, the performance of embodiment 1-4 are tested better than comparative example 1-2, especially precipitation analyte detection, toughness of material test and smell
Test result is more excellent, it was demonstrated that of the invention to blend together resistance in advance using PA6 toner (80~200 mesh number) and MCA fire retardant
Fire agent powder packet, and using side feed charging by the way of, to obtain the low precipitation fire-retardant polyamide material of low smell, and material tool
There are good flame retardant effect and toughness.The smell of embodiment 1-4 is surveyed it can be seen from 3 correlation data of embodiment 1-4 and comparative example
Test result is substantially better than comparative example 3, it was demonstrated that and it is of the invention that fire-retardant polyamide material is prepared using black soy sauce vacuum double screw extruder,
Good odor effect can be obtained.The smell of embodiment 1-4 is surveyed it can be seen from 4 correlation data of embodiment 1-4 and comparative example
Examination, flame retardant test and toughness test are superior to comparative example 4, it was demonstrated that of the invention using compounding eliminating smell agent (partial size≤15 μm D99)
Show good taste removal adsorption effect, flame retardant property and toughness of material.It can be seen that Compositional type by above embodiments data
There is the double screw extruder of black soy sauce vacuum to prepare fire-retardant polyamide material for the addition and use of eliminating smell agent, keep material tough
Property and while flame retardant effect, the oder levels of material can be obviously improved, performance and mold deposits performance is precipitated.
The skilled worker of the industry it should be appreciated that the present invention is not limited by above-mentioned implementing regulations, above-mentioned implementing regulations and
It is only intended to illustrate the principle of the present invention described in specification, under the premise of not departing from the present invention and range, the present invention is also
There can be various changes and modifications, these changes and improvements belong in scope of the claimed invention.It is claimed
Range is the same as appended claims and other equivalent thereofs.
Claims (9)
1. a kind of low precipitation fire-retardant polyamide material of low smell, which is characterized in that be grouped as by the group of following weight percent meter:
Polyamide: 84.5%~92%；
Fire retardant: 7%~13%；
Eliminating smell agent: 0.5%~1.5%；
Lubricant: 0.3%~0.5%；
Antioxidant: 0.2%~0.5%；
Wherein, the fire retardant is melamine cyanurate (MCA) fire retardant；
The eliminating smell agent is the composition of organic zinc salt and Si-Al molecular sieve；Organic zinc salt is can response type Long carbon chain organic zinc
Salt；Si-Al molecular sieve has porous structure；Partial size D99≤15 μm of Si-Al molecular sieve.
2. the low precipitation fire-retardant polyamide material of low smell according to claim 1, which is characterized in that the polyamide includes
Nylon66 fiber (PA66) resin slicer and nylon 6 (PA6) toner；Nylon 66 resin be sliced relative viscosity (R.V.) be 2.4~
2.8；Nylon 6 resin powder relative viscosity is 2.4~2.8；Nylon 66 resin slice and nylon 6 resin powder weight ratio be 7~
10:0.5~1；Nylon 6 resin powder is the powdex of 80~200 mesh partial sizes.
3. the low precipitation fire-retardant polyamide material of low smell according to claim 1, which is characterized in that the melamine cyanogen
Partial size D99≤50 μm of lithate fire retardant.
4. the low precipitation fire-retardant polyamide material of low smell according to claim 1, which is characterized in that the lubricant is hard
One or more of resin acid salt, ethylene acrylic acid co polymer and amide series lubricant agent.
5. the low precipitation fire-retardant polyamide material of low smell according to claim 1, which is characterized in that the antioxidant be by
Hinder one or more of phenols primary antioxidant, phosphorous acid esters auxiliary anti-oxidant.
6. the low preparation method that fire-retardant polyamide material is precipitated of one kind low smell according to any one of claims 1 to 5,
It is characterized in that, comprising the following steps:
Step 1 puts into first part's polyamide and fire retardant in high-speed mixer, is uniformly mixed, and fire retardant powder is made
Packet, it is spare；
Step 2 puts into eliminating smell agent, lubricant and antioxidant in low-speed mixer, is uniformly mixed, and auxiliary agent packet is made, spare；
Step 3 feeds intake auxiliary agent packet made from second part polyamide and step 2 from the main spout of double screw extruder；It will
Fire retardant powder packet made from step 1 individually feeds intake from the side spout of double screw extruder；It squeezes out, water cooling is crossed, after pelletizing
The low precipitation fire-retardant polyamide material of low smell is made.
7. the low preparation method that fire-retardant polyamide material is precipitated of low smell according to claim 6, which is characterized in that step
Double screw extruder in 3 has black soy sauce vacuum function.
8. the low preparation method that fire-retardant polyamide material is precipitated of low smell according to claim 6, which is characterized in that step
First part's polyamide in 1 is nylon 6 resin powder；Second part polyamide in step 3 is nylon 66 resin slice.
9. the low application that fire-retardant polyamide material is precipitated of one kind low smell according to any one of claims 1 to 5, feature
It is, the low precipitation fire-retardant polyamide material of the low smell is used as automotive electronics electrical equipment material.
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| CN113025035A (en) * | 2021-04-12 | 2021-06-25 | 东莞市东翔塑胶有限公司 | Laser-markable halogen-free flame-retardant nylon composite material and preparation method thereof |
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| CN113524623A (en) * | 2021-06-01 | 2021-10-22 | 金旸（厦门）新材料科技有限公司 | Method for improving impact performance of MCA flame-retardant PA66 |
| CN114213838A (en) * | 2021-12-03 | 2022-03-22 | 上海金发科技发展有限公司 | Flame-retardant nylon composite material with low pungent smell and preparation method and application thereof |
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