CN107383864A - A kind of reinforced polyamide/polyolefin alloy material and preparation method thereof - Google Patents
A kind of reinforced polyamide/polyolefin alloy material and preparation method thereof Download PDFInfo
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- 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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L23/06—Polyethene
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
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- 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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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2207/06—Properties of polyethylene
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- C08L2312/00—Crosslinking
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Abstract
The present invention relates to a kind of reinforced polyamide/polyolefin alloy material and preparation method thereof, the alloy material includes the composition of following parts by weight：20~100 parts of polyamide；0~80 part of polyolefin；35~70 parts of filler；1~15 part of sensitizer；0.2~2 part of nucleator；0~20 part of fire retardant；1~6 part of coupling agent；0~20 part of compatilizer, during preparation, first coupling agent is pre-processed, polyamide, polyolefin, filler, sensitizer, coupling agent and compatilizer are uniformly mixed by weight, pre-composition is made, extruder then is shifted into premixing, side adds fire retardant, filler by weight, it is granulated and dries, you can obtains product.Compared with prior art, material dose of radiation of the present invention is low, temperature resistant grade is high, good stability of the dimension, cost are low, efficiently solve poor dimensional stability after nylon material absorbs water, brittle failure caused by nylon water absorption rate is low in microthermal climate dry environment, high-temperature material even can be replaced in the not high occasion of some mechanical property requirements, greatly reduces cost.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of reinforced polyamide/polyolefin alloy material and its
Preparation method.
Background technology
Polyamide (being commonly called as nylon) is that yield is maximum, kind is most, one of most widely used engineering plastics.With automobile work
The development in the fields such as industry, electric, communications and transportation, machinery, Aero-Space and various dairy industries, has significantly promoted polyamide
Research, production and application, be greatly promoted polyamide kind variation and performance improvement and raising.However, due to
Amide group in polyamide molecule has water imbibition, so the water suction of polyamide material is generally higher, it is poly- after absorbing water
Acid amides has obvious reduction in terms of mechanical strength, metal adhesion, and this also greatly hinders the popularization and application of polyamide.
Polyolefin (PO, Polyolefin) is the total of polyethylene, polypropylene and poly 1-butene and other olefin polymers
Claim.For world wide, the yield of polyolefin accounts for the nearly half of synthetic resin total amount.It is close with national economy and people's lives
Correlation, its yield number turned into the important symbol of National Industrial up-to-dateness.It is that modern petrochemical industry is most important
Product, be again plastic products primary raw material.
Application No. 201110044529.X Chinese invention patent discloses a kind of crosslinking with radiation halogen-free flame-retardant polyamide
CABLE MATERIALS and preparation method and application, described sensitizer are trimethylolpropane trimethacrylate, trimethylolpropane tris
Methacrylate, pentaerythritol triacrylate, dose of radiation 90kGy is bigger than our existing technique dose of radiations, and
And we did actual DSC and gel test, the product after radiation is not crosslinking.
The Chinese invention patent of Application No. 201010223859.0 discloses a kind of wear-resistant self-lubricating nylon compound material
And preparation method thereof, described sensitizer is isocyanide urea triallyl, trimethylolpropane trimethacrylate, and dose of radiation is
90kGy~120kGy, bigger than our existing technique dose of radiations, similar with a upper patent, our actual test shows,
Trimethylolpropane trimethacrylate, trimethylol-propane trimethacrylate, pentaerythritol triacrylate, isocyanide urea three
Allyl ester can only all trigger the crosslinking with radiation of polyolefin, at least dose of radiation our existing process parameter 70kGy (cobalt source) with
When lower, the nylon product of crosslinking can not be actually obtained.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of good stability of the dimension,
Wide reinforced polyamide/polyolefin alloy material of use temperature range and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：A kind of reinforced polyamide/polyolefin alloy material,
The alloy material includes the composition of following parts by weight：
Toughness becomes strong after nylon water suction, but can expand, and accessory size precision is not high.And if do not absorbed water, toughness is not
It is enough, for example when winter (low temperature, low humidity), nylon part is just easy to that brittle fracture occurs and fails.The present invention uses
Polyamide/polyolefin alloy system, and crosslinking with radiation is carried out to alloy material, the benefit done so includes：First, polyolefin
Addition, substantially improve the low temperature impact properties of polyamide nylon；Second, radiation can introduce oxygen original on the main chain of polyolefin
Son, polarity is improved, add the compatibility of polyamide and polyolefin；3rd, by that with when technique, polyolefin can be made and gathered
Acid amides forms two-arch tunnel structure, and interpenetrating networks (IPN) can be formed by crosslinking with radiation, and barrier is extremely strong, and water absorption rate is extremely low,
Solves the shortcomings that size is unstable after nylon absorbs water.
Described polyamide includes one in PA6, PA66, PA610, PA11, PA12, PA1010, PA1012 or PA1212
Kind is a variety of.
Described polyolefin includes the one or more in LDPE, LLDPE, HDPE, POE, EPDM, SBS or SEBS.
Described filler includes short glass fiber or montmorillonite, the draw ratio of the short glass fiber for 50~
200, vinyl acetate organic-treating is passed through in the montmorillonite.
Described sensitizer is selected from penylene BMI, N between triallyl cyanurate, N, N'-, N- (4- methyl isophthalic acids,
3- phenylenes) BMI or N, N'- (4,4'- methylenediphenyls) BMI one or more.Its
In, triallyl cyanurate is the crosslinking sensitizer of polyolefin, the crosslinking with radiation effect of its energy efficient hardening polyolefin polymers
Fruit.(4,4'- is sub- by penylene BMI, N between N, N'-, N- (4- methyl isophthalic acids, 3- phenylenes) BMIs and N, N'-
Methyldiphenyl base) BMI structural formula it is as follows：
Three belongs to BMI based sensitisers, BMI based sensitisers very radiation hardness in itself.In spoke
When penetrating dosage and reaching 100kGy, still not autohemagglutination is not crosslinked.But when being added in nylon, under radiation condition, drawn by ray
The nylon free radical of hair can lure that the double bond of BMI based sensitisers is opened into, and the radiation for participating in and strengthening nylon is handed over
Connection.
During due to crosslinking with radiation, the crystallinity of polymer is improved, is unfavorable for the progress of cross-linking reaction, in addition, crystallization also presses down
The cracking of segment is made, and the degree suppressed is bigger.Due to free radical can also be caught on the surface of crystalline region, it is seen that increase ball
Brilliant specific surface area (for example reducing spherulite size), under conditions of same crystallinity, final gel content is more.In addition, by
There is obvious radiation aftereffect in the sensitizer of bismaleimide amine, have plus early stage in order to strengthen cross-linking effect, during shaping
Anticipate the cerium sulphate crystal of part at one than relatively low level, so needing to anneal to part after radiation.
Described nucleator is powdery neodymium oxide.Nucleator can be effectively increased the specific surface area of crystal, there is provided more
More cross-linking reaction places.
The one kind or more of the fire retardant in poly- bromostyrene, antimony oxide, phosphinates, capsule red phosphorus
Kind, the coupling agent be selected from KR-TTS, KH550, KH560 one or more, the compatilizer be selected from LDPE-g-MAH,
HDPE-g-MAH, SBS-g-MAH one kind.
A kind of preparation method of reinforced polyamide/polyolefin alloy material as described above, comprises the following steps：
(1) coupling agent is handled in advance, then by weight by polyamide, polyolefin, filler, coupling agent, quick
Agent, nucleator and compatilizer mixing, stir, pre-composition are made；The filler added in the step is montmorillonite, if production
Montmorillonite is not used in product, then is added without filler in the step；
(2) pre-composition is transferred in extruder, adds fire retardant and filler by weight during extrusion, make
Grain, to dry, produce the reinforced polyamide/polyolefin alloy material, the filler added in the step is short glass fiber,
If not containing short glass fiber in final product, filler is not added in the step.
Described coupling agent includes KR-TTS, KH550, KH560 one or more, when in coupling agent contain KH550 or
KH560, the processing of coupling agent is hydrolysis or alcoholysis, i.e., coupling agent is configured into the aqueous solution or alcohol that mass concentration is 10~50%
Solution, and it is 4.0~5.5 to control solution ph；
When containing KR-TTS in coupling agent, the processing of coupling agent is by KR-TTS and atoleine 1:2 mixing.To coupling
Agent is pre-processed, be in order that coupling agent is scattered more uniform.
Described extruder is double screw extruder, and the process conditions of granulation are area's temperature：90~160 DEG C, 2nd area：
180~260 DEG C, 3rd area：210~260 DEG C, 4th area：220~260 DEG C, 5th area：220~260 DEG C, 6th area：220~260 DEG C, seven
Area：220~260 DEG C, die head temperature：220~260 DEG C.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects：
(1) by the alloy system of polyamide/polyolefine, the low temperature impact properties of polyamide nylon have been can effectively improve,
And improve both compatibilities；
(2) by that with when technique, PA and PO can be made to form two-arch tunnel structure, can be formed mutually by crosslinking with radiation
Network (IPN) is worn, barrier is extremely strong, and water absorption rate is extremely low, solves the shortcomings that size is unstable after nylon absorbs water；
(3) by the sensitizer of the present invention, cooperateed with PA or PO, increase PA and PO crosslinking with radiation degree.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：100 parts of PA66,70 parts of short glass fiber, 15 parts of N, N'- (4,4'- methylenediphenyls) BMI,
Nd2O32 parts, 15 parts of poly- bromostyrene, 5 parts of antimony oxide, 6 parts of KH560.Dose of radiation：70kGy.
Embodiment 2：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：90 parts of PA1010,10 parts of LLDPE, 50 parts of short glass fiber, N, N'- (4,4'- methylenediphenyls) span come
10 parts of acid imide, 0.8 part of Nd2O3,15 parts of phosphinates, 4 parts of KH560,10 parts of LDPE-g-MAH.Dose of radiation：70kGy.
Embodiment 3：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：55 parts of PA6,45 parts of HDPE, 35 parts of short glass fiber, 25 parts of MMT, 1 part of TAC, N, N'- (4,4'- methylene
Diphenyl) 9 parts of BMI, 0.4 part of Nd2O3,1 part of KH550,1 part of KP-TTS, 20 parts of HDPE-g-MAH.Radiation
Dosage：70kGy.
Embodiment 4：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：(4,4'- is sub- by 65 parts of PA610,35 parts of LLDPE, 35 parts of short glass fiber, 25 parts of MMT, 1 part of TAC, N, N'-
Methyldiphenyl base) 9 parts of BMI, 0.6 part of Nd2O3,2 parts of KH550,1 part of KP-TTS, 15 parts of LDPE-g-MAH.
Dose of radiation：70kGy.
Embodiment 5：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：75 parts of PA11,25 parts of LDPE, 45 parts of short glass fiber, 2 parts of TAC, penylene BMI 8 between N, N'-
Part, 0.8 part of Nd2O3,3 parts of KH550,10 parts of POE-g-MAH.Dose of radiation：70kGy.
Embodiment 6：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：55 parts of PA1212,30 parts of HDPE, 15 parts of EPDM, 50 parts of short glass fiber, 20 parts of MMT, 1 part of TAC, N,
10 parts of N'- (4,4'- methylenediphenyls) BMI, 1 part of Nd2O3,1.5 parts of KH550 KH550, KP-TTS 0.5
Part, 15 parts of HDPE-g-MAH.Dose of radiation：70kGy.
Embodiment 7：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：80 parts of PA1010,5 parts of LLDPE, 15 parts of POE, 60 parts of short glass fiber, 1 part of TAC, N, N- (4- methyl isophthalic acids,
3- phenylenes) 12 parts of BMI, 1.6 parts of Nd2O3,2 parts of KH550.Dose of radiation：70kGy.
Embodiment 8：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：(4- methyl isophthalic acids, 3- are sub- by 70 parts of PA12,5 parts of SBS, 15 parts of POE, 60 parts of short glass fiber, 1 part of TAC, N, N-
Phenyl) 12 parts of BMI, 1.2 parts of Nd2O3,2 parts of KH550,5 parts of SBS-g-MAH.Dose of radiation：70kGy.
Embodiment 9：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：20 parts of PA6,80 parts of HDPE, 50 parts of short glass fiber, 20 parts of MMT, 1 part of TAC, 0.2 part of Nd2O3, KH550
2 parts, 2 parts of KR-TTS.Dose of radiation：70kGy.
Embodiment 10：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：90 parts of PA612,10 parts of SEBS, 40 parts of short glass fiber, 1 part of TAC, N, N'- (4,4'- methylenediphenyls)
14 parts of BMI, 1 part of Nd2O3,15 parts of red phosphorus, 2 parts of KH550.Dose of radiation：70kGy.
Embodiment 11：
The present embodiment glass-fiber-reinforced polyamide/polyolefin alloy material is by including the component system of following parts by weight content
It is standby to form：50 parts of PA66,50 parts of PA6,60 parts of short glass fiber, N, N'- (4,4'- methylenediphenyls) bismaleimide
20 parts of amine, 1 part of Nd2O3,1 part of KH560,1 part of KH550.Dose of radiation：70kGy.
The preparation technology flow of 1~embodiment of embodiment 11 is identical, comprises the following steps that：
(1) in advance by silane coupler be configured to mass concentration be 10~50% ethanol solution, and adjust pH to 4.0~
5.5, by titanate coupling agent and atoleine 1:2 mixing, then by weight by polyamide, polyolefin, MMT, coupling agent, quick
Agent, nucleator and compatilizer mixing, stir, pre-composition are made；
(2) pre-composition is transferred in double screw extruder, adds fire retardant and glass by weight during extrusion
Glass fiber, it is granulated, dries, produce the reinforced polyamide/polyolefin alloy material.The process conditions being wherein granulated are area's temperature
Degree：90~160 DEG C, 2nd area：180~260 DEG C, 3rd area：210~260 DEG C, 4th area：220~260 DEG C, 5th area：220~260 DEG C,
6th area：220~260 DEG C, 7th area：220~260 DEG C, die head temperature：220~260 DEG C.
The difference of the polyamide used according to 1~embodiment of embodiment 11, annealed after carrying out radiation treatment to product,
Annealing conditions are as follows according to the difference of polyamide：
| Polymer | Fusing point (K) | Annealing temperature (K) | Annealing time (hr) | Remarks |
| PA6 | 502 | 413 (~140 DEG C) | 0.5~1.0 | Existing document is delivered |
| PA11 | 466 | 373 (~100 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA12 | 451 | 361 (~88 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA66 | 538 | 420 (~147 DEG C) | 0.5~1.0 | Existing document is delivered |
| PA610 | 493 | 394.5 (~121.4 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA612 | 485 | 388 (~115 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA1010 | 477 | 382 (~108.6 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA1012 | 467 | 374 (~100.6 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
| PA1212 | 456 | 365 (~92 DEG C) | 0.5~1.0 | Estimated by Tm*0.8 |
The alloy material of the gained of 1~embodiment of embodiment 11 is detected with control group, wherein, example 1, example 11 should
In guide plate for electrothermal relay product, test foundation is shown in 8.2.1.5.1.1e in GBT 14048.4) part.As a result it is as follows：
Material obtained by example 3, example 4, example 6 has an IPN structures, and water absorption rate is extremely low after part cross-linking radiation,
It is very suitable for being applied to the high occasion of required precision.Here is applied in miniature circuit breaker, and the excess of stroke is surveyed after long delay experiment
As a result：
Example 2, example 5, example 7, example 8, example 10, material at low temperature impact strength is good, applied in A.C. contactor,
Contrasted with the material used originally：
Claims (10)
1. a kind of reinforced polyamide/polyolefin alloy material, it is characterised in that the alloy material includes the group of following parts by weight
Into：
A kind of 2. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that described polyamides
Amine includes the one or more in PA6, PA66, PA610, PA11, PA12, PA1010, PA1012 or PA1212.
A kind of 3. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that described polyene
Hydrocarbon includes the one or more in LDPE, LLDPE, HDPE, POE, EPDM, SBS or SEBS.
A kind of 4. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that described filling
Agent includes the one or more in short glass fiber or montmorillonite, and the draw ratio of the short glass fiber is 50~200, institute
State montmorillonite and pass through vinyl acetate organic-treating.
A kind of 5. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that described sensitization
Agent is selected from penylene BMI, N, N- (4- methyl isophthalic acids, 3- phenylenes) span between triallyl cyanurate, N, N'- and carrys out acyl
The one or more of imines or N, N'- (4,4'- methylenediphenyls) BMI.
A kind of 6. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that described nucleation
Agent is powdery neodymium oxide.
A kind of 7. reinforced polyamide/polyolefin alloy material according to claim 1, it is characterised in that the fire retardant
One or more in poly- bromostyrene, antimony oxide, phosphinates, capsule red phosphorus, the coupling agent are selected from KR-
TTS, KH550, KH560 one or more, the compatilizer are selected from the one of LDPE-g-MAH, HDPE-g-MAH, SBS-g-MAH
Kind.
8. a kind of preparation method of reinforced polyamide/polyolefin alloy material as described in claim 1~7 is any, its feature exist
In comprising the following steps：
(1) coupling agent is handled in advance, then by weight by polyamide, polyolefin, filler, coupling agent, sensitizer,
Nucleator and compatilizer mixing, stir, pre-composition are made；
(2) pre-composition is transferred in extruder, adds fire retardant and filler by weight during extrusion, be granulated,
Dry, produce the reinforced polyamide/polyolefin alloy material.
A kind of 9. preparation method of reinforced polyamide/polyolefin alloy material according to claim 8, it is characterised in that
Described coupling agent includes KR-TTS, KH550, KH560 one or more, when containing KH550 or KH560 in coupling agent, occasionally
The processing for joining agent is hydrolysis or alcoholysis, i.e., coupling agent is configured into the aqueous solution or alcoholic solution that mass concentration is 10~50%, and
It is 4.0~5.5 to control solution ph；
When containing KR-TTS in coupling agent, the processing of coupling agent is by KR-TTS and atoleine 1:2 mixing.
A kind of 10. preparation method of reinforced polyamide/polyolefin alloy material according to claim 8, it is characterised in that
Described extruder is double screw extruder, and the process conditions of granulation are area's temperature：90~160 DEG C, 2nd area：180~260
DEG C, 3rd area：210~260 DEG C, 4th area：220~260 DEG C, 5th area：220~260 DEG C, 6th area：220~260 DEG C, 7th area：220~
260 DEG C, die head temperature：220~260 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710853033.4A CN107383864A (en) | 2017-09-20 | 2017-09-20 | A kind of reinforced polyamide/polyolefin alloy material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710853033.4A CN107383864A (en) | 2017-09-20 | 2017-09-20 | A kind of reinforced polyamide/polyolefin alloy material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330787A (en) * | 2019-07-04 | 2019-10-15 | 四川轻化工大学 | A kind of preparation method of linear low density polyethylene graft modification of nylon 6 |
| CN112876841A (en) * | 2021-01-15 | 2021-06-01 | 万华化学(四川)有限公司 | Halogen-free flame-retardant long glass fiber reinforced nylon 12 material with high RTI value as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330787A (en) * | 2019-07-04 | 2019-10-15 | 四川轻化工大学 | A kind of preparation method of linear low density polyethylene graft modification of nylon 6 |
| CN112876841A (en) * | 2021-01-15 | 2021-06-01 | 万华化学(四川)有限公司 | Halogen-free flame-retardant long glass fiber reinforced nylon 12 material with high RTI value as well as preparation method and application thereof |
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Application publication date: 20171124 |