CN106496452A - A kind of toughener, ultra-toughness PBT and preparation method thereof - Google Patents
A kind of toughener, ultra-toughness PBT and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F287/00—Macromolecular compounds obtained by polymerising monomers on to block polymers
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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
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92514—Pressure
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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
- B29C2948/92—Measuring, controlling or regulating
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- B29C2948/92704—Temperature
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of toughener, ultra-toughness PBT and preparation method thereof, material proportioning by weight is：70～96 parts of PBT polybutylene terephthalate (PBT)s resin；2～10 parts of PC polycarbonate resins；2～20 parts of toughener, wherein toughener are that self-control GMA (GMA) and methyl methacrylate (MMA) dual graft SEBS, its proportioning by weight are：82～97 parts of SEBS；2～10 parts of co-monomer；0.1～0.2 part of initiator；1～2 part of GMA；1～2 part of MMA.The present invention had both been maintained the intensity of PBT material, had been effectively improved the toughness of PBT again by design and processes control of filling a prescription, the low-temperature impact effect of the PBT material being greatly enhanced, household electrical appliance are can be widely applied to, electric and automobile, the field such as consumer goods industries.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to a kind of toughener, ultra-toughness PBT and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT), abbreviation PBT is that milky is translucent to opaque, crystal type thermoplastic resin.
The features such as there is high-fire resistance, fatigue durability, self-lubricating, low-friction coefficient, weatherability.Its water absorption rate is low, and only 0.1%,
Various physical property (including electrical property) are still kept in wet environment.
The notch impact strength of common PBT is not high, in engineering plastics application, mainly glass fibre reinforced modified is
Main, resistant to elevated temperatures industrial product is needed for automobile, electronic apparatus, industrial machinery etc..Distributor, car in such as automobile
Such as TV during body component, ignitor coil skeleton, insulating lid, gas extraction system parts, motor cycle ignitor, electronic apparatus are industrial
The deflection coil of machine, kinescope and potentiometer support, sound accompaniment output transformer framework, adapter skeleton, switch connector, etc.
Deng.
Pure PBT is used for the application of toughening modifying and be not as extensive as nylon and PC, and main cause is the toughness reinforcing common with market
Agent and some modified gimmicks existing, toughening effect are simultaneously unsatisfactory, and particularly the low-temperature impact-resistant situation of material improves and has
Limit.After toughener is excessively added, loss of strength is excessive, and product is more difficult to popularization and application.
Content of the invention
It is an object of the invention to provide a kind of ultra-toughness PBT and preparation method thereof, can be effectively improved the impact resistance of PBT material
Energy, particularly low-temperature impact-resistant performance, greatly expand the range of application of PBT material.
Another object of the present invention is to provide a kind of excellent toughener and preparation method thereof, is suitable to produce ultra-toughness PBT material.
In order to realize foregoing invention purpose, technical scheme is as follows：
A kind of toughener, its constitute proportioning by weight be：
Preferably, the co-monomer is styrene；The initiator is benzene cumyl peroxide DCP.
A kind of preparation method of toughener as above, including step：
1) proportioning weighs each component by weight；
2) GMA and MMA in the component is dissolved in the middle of co-monomer, then is placed in high mixer with SEBS and initiator and stirs
Mix 5-10 minutes；
3) mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area
140～170 DEG C of temperature, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head
170～210 DEG C of temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure
A kind of ultra-toughness PBT material, its constitute proportioning by weight be：
70～96 parts of PBT；
2～10 parts of PC；
2～20 parts of toughener；
The compatilizer is toughener described above.
Above-mentioned ultra-toughness PBT is further comprising the filler or fire retardant for accounting for 20～50 parts of parts by weight.
The filler be glass fibre, talcum powder, kaolin, calcium carbonate, barium sulfate, the one kind or several in titanium dioxide
Kind, the fire retardant be brominated epoxy, brominated polycarbonate, brominated Polystyrene, brominated triazine, TDE, three oxygen
Change two antimony, Firebrake ZB, ethylphosphinic acid salt, red phosphorus etc. one or more.
A kind of preparation method of ultra-toughness PBT as above, including step：
a：Proportioning weighs each component by weight；
b：To stir 5-20 minutes in the described group of high mixer that is placed in；
c：The mixture obtained in step b is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area
190～210 DEG C of temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, head
210～240 DEG C of temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
The present invention by make by oneself toughener, its have high percent grafting with high low temperature resistant the characteristics of, be the excellent toughness reinforcings of PBT
Agent.The ultra-toughness PBT material for preparing, had both maintained the intensity of PBT material, is effectively improved the toughness of PBT again, greatly carries
The low-temperature impact effect of high PBT material, can be widely applied to household electrical appliance, electric and automobile, consumer goods industries etc.
Field..
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect become more apparent, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only in order to explain the present invention
Limit the present invention.
A kind of ultra-toughness PBT material, its constitute proportioning by weight be：
70～96 parts of PBT；
2～10 parts of PC；
2～20 parts of toughener；
The addition of wherein PC (Merlon), can play a part of increase-volume and supplement intensity.
Further, filler or fire retardant comprising 20～50 parts by weight；
Glass fibre, talcum powder, kaolin, calcium carbonate, barium sulfate, one or more in titanium dioxide, the fire retardant
For brominated epoxy, brominated polycarbonate, brominated Polystyrene, brominated triazine, TDE, antimony oxide, Firebrake ZB,
Ethylphosphinic acid salt, red phosphorus etc. one or more.Addition filler is modified plastics common method, can improve the mechanicalness of material
Energy and heat resistance, preferably glass fibre.Add fire retardant improve the fire protecting performance of material, preferably bromo- antimony compounding, such as
Brominated epoxy resin is used cooperatively with antimony oxide.
And, above-mentioned ultra-toughness PBT material, including following preparation process：
1. formula as requested weighs each component respectively；
2. will stir 5-20 minutes in the described group of high mixer that is placed in；
3. by step 2. in the mixture that obtains be placed in dual-screw-stem machine, through melting extrusion, granulate, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Meanwhile, the toughener adopted by above-mentioned ultra-toughness PBT material is self-control GMA and MMA dual graft SEBS.Its composition is pressed
Parts by weight proportioning is：
Wherein, SEBS can be as the main body of toughener, with splendid toughened cold-resistant effect.
Above-mentioned GMA and MMA are highly polar reactive groups, are a kind of macromolecule interfacial coupling agent, compatilizer, dispersion
Accelerator.Wherein GMA is easily reacted with PBT ends, can improve the compatibility performance of PBT and SEBS.And MMA groups are then not only
Can react with PBT ends, PBT can be substantially increased, the compatibility between PC and SEBS to react with PC ends.
Above-mentioned co-monomer be styrene, styrene one side melting be grafted auxiliary agent GMA and MMA, improve melt processability,
Play and help scattered effect；On the other hand can then suppress the decomposition of SEBS materials, improve the percent grafting of graft reaction.
Above-mentioned initiator is benzene cumyl peroxide DCP, can be catalyzed initiation GMA and MMA and be grafted in SEBS strands.
And, above-mentioned self-control toughener GMA and MMA dual graft SEBS is comprised the following steps：
1) proportioning weighs each component by weight；
2) GMA and MMA in the component is dissolved in the middle of co-monomer, then is placed in high mixer with SEBS and initiator and stirs
Mix 5-10 minutes；
3) mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area
140～170 DEG C of temperature, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head
170～210 DEG C of temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure
Below by taking the concrete ultra-toughness PBT material formula and preparation method as an example, the present invention will be described in further detail.
The preparation of toughener：
Embodiment A
The present invention first prepares toughener GMA and MMA Maleated SEBS, and its composition proportioning by weight is：
GMA and MMA in the component is dissolved in the middle of co-monomer, then stirring in high mixer is placed in SEBS and initiator
5-10 minutes；
The mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area's temperature
140～170 DEG C of degree, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head temperature
170～210 DEG C of degree material, the cylinder time of staying is 1～2 minute, and 10～20MPa of melt pressure finally gives GMA and MMA dual grafts
SEBS toughener.
Embodiment B
Toughener its constitute proportioning by weight be：
The present invention first prepares toughener GMA and MMA Maleated SEBS, and its composition proportioning by weight is：
GMA and MMA in the component is dissolved in the middle of co-monomer, then stirring in high mixer is placed in SEBS and initiator
5-10 minutes；
The mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area's temperature
140～170 DEG C of degree, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head temperature
170～210 DEG C of degree material, the cylinder time of staying is 1～2 minute, and 10～20MPa of melt pressure finally gives GMA and MMA dual grafts
SEBS toughener.
Embodiment C
Toughener its constitute proportioning by weight be：
The present invention first prepares toughener GMA and MMA Maleated SEBS, and its composition proportioning by weight is：
GMA and MMA in the component is dissolved in the middle of co-monomer, then stirring in high mixer is placed in SEBS and initiator
5-10 minutes；
The mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area's temperature
140～170 DEG C of degree, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head temperature
170～210 DEG C of degree material, the cylinder time of staying is 1～2 minute, and 10～20MPa of melt pressure finally gives GMA and MMA dual grafts
SEBS toughener.
The preparation that compatilizer obtained above is used for PPSU and PEEK alloys, concrete example are as follows：
Embodiment 1
The formula of as requested weighs each component respectively；
97 parts of PBT；
3 parts of PC；
4 parts of toughener；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Embodiment 2
The formula of as requested weighs each component respectively；
82 parts of PBT；
8 parts of PC；
15 parts of toughener；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Embodiment 3
The formula of as requested weighs each component respectively；
87 parts of PBT；
5 parts of PC；
8 parts of toughener；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Embodiment 4
The formula of as requested weighs each component respectively；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Comparative example 1
Comparative example makees reference using commercially available French A Ke agates toughener AX8900, and formula on request claims respectively
Take each component；
92 parts of PBT；
8 parts of AX8900；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Comparative example 2
The formula of as requested weighs each component respectively；
87 parts of PBT；
5 parts of PC；
8 parts of toughener；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Comparative example 3
The formula of as requested weighs each component respectively；
To stir 5-20 minutes in the described group of high mixer that is placed in；
The mixture obtained in above step is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One
190～210 DEG C of area's temperature, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, machine
210～240 DEG C of head temperature material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
Performance test is tested：
The particle for completing as stated above is dried in 120 DEG C of convection oven 3-6 hours in advance, then again will be dry
Dry good particulate material carries out injection moulding sample preparation in injector, and injection moulding die temperance control is at 120 DEG C.
Tensile strength test is carried out by ASTM D638 standards, and specimen size is 180 × 12.7 × 3.2mm, and draw speed is
50mm/min；Bending strength is carried out by ASTM D790 standards, and rate of bending is 3mm/min, and specimen size is 128mm × 13mm
×3.2mm；Cantilever beam impact strength is carried out by ASTM D256 standards, specimen size be 63.5 × 12.7 × 4.2mm, breach chi
Very little for 1/5th of sample thickness；
The result of indices performance test sees below table 1.
Table 1
Compare with comparative example from embodiment, with the addition of the formula system of self-control toughener, than commercially available toughener with cube
System, its mechanical strength, toughness, particularly low-temperature impact-resistant intensity all have greatly improved, and illustrate to make by oneself toughener to PBT's
Toughened cold-resistant effect is very excellent.
In sum, the present invention had both maintained the intensity of PBT material by design and processes control of filling a prescription, and effectively
The toughness of PBT is improve, the low-temperature impact effect of the PBT material being greatly enhanced can be widely applied to household electrical appliance, electronics electricity
The fields such as gas and automobile, consumer goods industries.
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the present invention, all in essence of the invention
Any modification, equivalent and improvement that is made within god and principle etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of toughener, it is characterised in which constitutes proportioning by weight and is：
2. toughener as claimed in claim 1, it is characterised in that：The co-monomer is styrene.
3. toughener as claimed in claim 1, it is characterised in that：The initiator is benzene cumyl peroxide DCP.
4. a kind of power 1 as described in toughener preparation method, it is characterised in that including step：
1) proportioning weighs each component by weight；
2) GMA and MMA in the component is dissolved in the middle of co-monomer, then stirring 5- in high mixer is placed in SEBS, initiator
10 minutes；
3) mixture obtained in step 2 is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area's temperature
140～170 DEG C, two 150～190 DEG C of area's temperature, three 160～200 DEG C of area's temperature, four 150～190 DEG C of area's temperature, head temperature
170～210 DEG C of material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
5. a kind of ultra-toughness PBT material, it is characterised in which constitutes proportioning by weight and is：
70～96 parts of PBT；
2～10 parts of PC；
2～20 parts of toughener；
The toughener is the toughener described in any one of claim 1-4.
6. ultra-toughness PBT material as claimed in claim 5, it is characterised in that further comprising accounting for 20～50 parts of parts by weight
Filler or fire retardant.
7. ultra-toughness PBT material as claimed in claim 6, it is characterised in that the filler is glass fibre, talcum powder is high
Ridge soil, calcium carbonate, barium sulfate, one or more in titanium dioxide, the fire retardant be brominated epoxy, brominated polycarbonate, bromine
Change polystyrene, brominated triazine, TDE, antimony oxide, Firebrake ZB, ethylphosphinic acid salt, red phosphorus etc. a kind of or
Several.
8. a kind of power 5 as described in ultra-toughness PBT material preparation method, it is characterised in that including step：
a：Proportioning weighs each component by weight；
b：To stir 5-20 minutes in the described group of high mixer that is placed in；
c：The mixture obtained in step b is placed in dual-screw-stem machine, through melting extrusion, is granulated, process conditions are：One area's temperature
190～210 DEG C, two 200～230 DEG C of area's temperature, three 210～240 DEG C of area's temperature, four 200～230 DEG C of area's temperature, head temperature
210～240 DEG C of material, the cylinder time of staying are 1～2 minute, 10～20MPa of melt pressure.
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| CN108276742A (en) * | 2017-12-29 | 2018-07-13 | 江阴济化新材料有限公司 | A kind of modified PBT material and its preparation method and application |
| CN108752829A (en) * | 2018-07-18 | 2018-11-06 | 合肥安力电力工程有限公司 | A kind of high mechanics modified SEBS material and preparation method thereof |
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| CN108250697A (en) * | 2017-12-29 | 2018-07-06 | 江阴济化新材料有限公司 | A kind of antistatic PBT material and its preparation method and application |
| CN108276742A (en) * | 2017-12-29 | 2018-07-13 | 江阴济化新材料有限公司 | A kind of modified PBT material and its preparation method and application |
| CN108752829A (en) * | 2018-07-18 | 2018-11-06 | 合肥安力电力工程有限公司 | A kind of high mechanics modified SEBS material and preparation method thereof |
| CN111484740A (en) * | 2020-05-26 | 2020-08-04 | 上海睿麒塑业有限公司 | Blending material adopting polyphenyl ester and PBO fiber to fill thermoplastic resin and preparation method thereof |
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Application publication date: 20170315 |