CN105949728A - Preparation method of thermoplastic polyester elastomer composite - Google Patents
Preparation method of thermoplastic polyester elastomer composite Download PDFInfo
- Publication number
- CN105949728A CN105949728A CN201610333948.8A CN201610333948A CN105949728A CN 105949728 A CN105949728 A CN 105949728A CN 201610333948 A CN201610333948 A CN 201610333948A CN 105949728 A CN105949728 A CN 105949728A
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- CN
- China
- Prior art keywords
- thermoplastic polyester
- polyester elastomer
- preparation
- tpee
- elastomer composite
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
Abstract
A preparation method of thermoplastic polyester elastomer composite is related to the technical field of material preparation and includes: placing thermoplastic polyest4er elastomer (TPEE) and graphene nano-sheets (GNS) or functionalized graphene nano-sheets (fGNS) in an internal mixer, and melting and blending to obtain the thermoplastic polyester elastomer composite. The thermoplastic polyester elastomer composite has excellent performance, is simple to manufacture and easy to use.
Description
Technical field
The present invention relates to technical field of material, be specifically related to the preparation of a kind of thermoplastic polyester elastomer composite
Method.
Background technology
Thermoplastic polyester elastomer (TPEE) is a member that thermoplastic elastomer (TPE) (TPE) family is new, owing to TPEE polyester is hard
Polarity, rigidity and the crystallinity of section so that it is there is good hot property and oil resistant, solvent resistance etc..Additionally due to polyester soft segment
There is relatively low glass transition temperature, thus material possesses again excellent ageing resistace and mechanical property.TPEE has concurrently excellent
Good melt stability, thermoplasticity and good processability, can use multiple thermoplasticity processing technique, and to a certain degree
On solve the difficult problem of the not reproducible utilization of rubber, fast development becomes a kind of green material.
While it is true, the mechanical property of thermoplastic polyester elastomer or not enough, have impact on its in some cases should
With.
Summary of the invention
It is an object of the present invention to provide the preparation method of the thermoplastic polyester elastomer composite with excellent mechanical performance.
Technical solution of the present invention one is: thermoplastic polyester elastomer (TPEE) and graphene nanometer sheet (GNS) are placed in banburying
Machine is extruded after melt blending, obtains thermoplastic polyester elastomer composite.
Technical solution of the present invention two is: by the graphene nanometer sheet (fGNS) of thermoplastic polyester elastomer (TPEE) and functionalization
It is placed in banbury and extrudes after melt blending, obtain thermoplastic polyester elastomer composite.
Graphene (GNS) is by the carbonaceous green wood of carbon atom tightly packed one-tenth monolayer bi-dimensional cellular shape lattice structure, has
Excellent mechanics, calorifics and electric property, shows huge application in electronic device, storage material and field of compound material
Potential, in addition graphene nanometer sheet can also carry out modification, obtains the modified Graphene with the more preferable compatibility
Nanometer sheet.
The inventive method one with TPEE and GNS thermoplastic polyester elastomer composite as raw material, method two with TPEE and
FGNS thermoplastic polyester elastomer composite is that raw material produces, and is all easy to industrialized production, makes simple, can obtain
There is the thermoplastic polyester elastomer composite of mechanical property, easy to use.
Further, such as the GNS that puts into very little, then performance is the best, and the GNS put into is too many, then can cause GNS excess
Waste, and performance can decline.Therefore, the mass ratio that feeds intake of currently preferred described TPEE and GNS be 1: 0.001～
0.1。
Further, such as the fGNS that puts into very little, then performance is the best, and the fGNS put into is too many, then can cause fGNS
Excess is wasted, and performance can decline.Therefore, the mass ratio that feeds intake of currently preferred described TPEE and fGNS is 1:
0.001～0.1.
Accompanying drawing explanation
Fig. 1 is a kind of thermoplastic polyester elastomer composite and the sample of preparation method using embodiment 1 method to prepare
Bar photo.
Fig. 2 is a kind of thermoplastic polyester elastomer composite and the sample of preparation method using embodiment 4 method to prepare
Bar photo.
Fig. 3 is a kind of thermoplastic polyester elastomer composite and the sample of preparation method using comparative example 1 method to prepare
Bar photo.
Detailed description of the invention
One, embodiment 1:
1, being placed in banbury by TPEE Yu GNS that mass ratio is 1: 0.001, controlling banbury temperature is 190 DEG C, rotor speed
It is 50 rpm, extrudes after melt blending 6 min, obtain TPEE Yu GNS thermoplastic polyester elastomer compound particle.
2, TPEE Yu GNS thermoplastic polyester elastomer compound particle use miniature injection machine is injected into as shown in Figure 1
Standard dog bone (32 mm × 2, mm × 4 mm) and the test for tensile property.
Injection technique is: barrel temperature 190 DEG C, mold temperature 35 DEG C, injection pressure 600 bar, dwell pressure 600
bar。
Two, embodiment 2 to 3:
Use step same as in Example 1, only change the rate of charge (see table) of TPEE Yu GNS.
Three, embodiment 4:
1, being placed in banbury by TPEE Yu fGNS that mass ratio is 1: 0.001, controlling banbury temperature is 190 DEG C, and rotor turns
Speed is 50 rpm, extrudes after melt blending 6 min, obtains TPEE Yu fGNS thermoplastic polyester elastomer compound particle.
2, TPEE Yu fGNS thermoplastic polyester elastomer compound particle use miniature injection machine is injected into as shown in Figure 1
Standard dog bone (32 mm × 2, mm × 4 mm) and the test for tensile property.
Injection technique is: barrel temperature 190 DEG C, mold temperature 35 DEG C, injection pressure 600 bar, dwell pressure 600
bar。
Special instruction: the graphene nanometer sheet (fGNS) of functionalization is the new group in the upper grafting of Graphene (GNS), real
Preparing graphite oxide initially with the Hummers method improved in testing, specific experiment step is as follows: under the conditions of ice-water bath, weighs
2g natural flake graphite joins in the there-necked flask equipped with 46 ml concentrated sulphuric acids, adds 1 g sodium nitrate, keeps mechanical agitation, then
It is slowly added to 6 g potassium permanganate, maintains temperature below 20 DEG C of reaction 2 h；Remove ice-water bath, be heated to 35 DEG C of reaction 1 h；Slowly
Add 92 mL deionized waters, maintain temperature to react 30 min at 98 DEG C；Reaction is diluted to 300 mL with warm water after terminating, and adds
Enter a certain amount of H2O2With 5% HCl, by centrifugal method, colloid washing (is used 5% BaCl to neutral2Solution detection supernatant,
Without white precipitate), then colloid is taken out and be dried 24 h as in baking oven 50 DEG C, obtain GO.Weigh a certain amount of graphite oxide
In beaker, add deionized water, after utilizing the ultrasonic 1h of cell pulverization instrument, with centrifuge with the centrifugation of 8000 r/min,
Then take supernatant liquid in there-necked flask, regulate solution PH 10 ~ 11 with ammonia, add a certain amount of hydrazine hydrate, anti-at 98 DEG C
Answer filtering and washing after 3 h, and filter cake is placed in 50 DEG C of dry 12 h in baking oven, obtain Graphene (GNS) and preserve stand-by.Weigh
200 mg graphite oxides, in three-necked bottle, add DMF 20mL, after ultrasonic 1h, add 5g MDI, continue ultrasonic 0.5 h, then
Add 2 mL catalyst DBTDL, 80o12 h are reacted under C.With the above-mentioned solution of the washing with acetone of 3 times of volumes, product is placed in baking
In case, 50 DEG C are dried 48 h, obtain the graphene nanometer sheet (fGNS) of functionalization.
Four, embodiment 5 to 6:
1, use step the same as in Example 4, only change the rate of charge (see table) of TPEE Yu fGNS.
2, the composite above each example made uses miniature injection machine to be injected into standard dumbbell also shown in FIG. 2
Type (32 mm × 2, mm × 4 mm).
Injection technique is: barrel temperature 190 DEG C, mold temperature 35 DEG C, injection pressure 600 bar, dwell pressure 600
bar。
Five, comparative example 1:
1, being directly placed in banbury by TPEE, controlling banbury temperature is 190 DEG C, and rotor speed is 50 rpm, melt blending 6
Extrude after min, obtain TPEE particle.
2, TPEE use miniature injection machine be injected into standard dog bone (32 mm × 2, mm × 4 mm) as shown in Figure 3
With the test for tensile property.
Injection technique is: barrel temperature 190 DEG C, mold temperature 35 DEG C, injection pressure 600 bar, dwell pressure 600
bar.Fig. 3 product is pure white shape.
Six, analyze:
Following table is the mechanical strength contrast table that above each example obtains batten.
As can be seen from the above table: the thermoplastic polyester elastomer composite made with TPEE and GNS and with TPEE and
The mechanical property of the thermoplastic polyester elastomer composite that fGNS makes is far above TPEE；The wherein mass ratio of TPEE Yu fGNS
It is the mechanical property of the composite that mass ratio is 1: 0.01 of composite significantly greater than TPEE Yu GNS of 1: 0.01, and
It is far longer than the mechanical property of TPEE.
Claims (6)
1. the preparation method of a thermoplastic polyester elastomer composite, it is characterised in that: by thermoplastic polyester elastomer and stone
Ink alkene nanometer sheet is placed in banbury to be extruded after melt blending, obtains thermoplastic polyester elastomer composite.
Preparation method the most according to claim 1, it is characterised in that: described thermoplastic polyester elastomer and graphene nanometer sheet
The mass ratio that feeds intake be 1: 0.001～0.1.
Preparation method the most according to claim 2, it is characterised in that: described thermoplastic polyester elastomer and graphene nanometer sheet
The mass ratio that feeds intake be 1: 0.01.
4. the preparation method of a thermoplastic polyester elastomer composite, it is characterised in that: by thermoplastic polyester elastomer's function
The graphene nanometer sheet changed is placed in banbury and extrudes after melt blending, obtains thermoplastic polyester elastomer composite.
Preparation method the most according to claim 5, it is characterised in that: described thermoplastic polyester elastomer and the stone of functionalization
The mass ratio that feeds intake of ink alkene nanometer sheet is 1: 0.001～0.1.
Preparation method the most according to claim 5, it is characterised in that: described thermoplastic polyester elastomer and the stone of functionalization
The mass ratio that feeds intake of ink alkene nanometer sheet is 1: 0.01～0.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333948.8A CN105949728A (en) | 2016-05-19 | 2016-05-19 | Preparation method of thermoplastic polyester elastomer composite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333948.8A CN105949728A (en) | 2016-05-19 | 2016-05-19 | Preparation method of thermoplastic polyester elastomer composite |
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Family
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| CN201610333948.8A Pending CN105949728A (en) | 2016-05-19 | 2016-05-19 | Preparation method of thermoplastic polyester elastomer composite |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008045778A1 (en) * | 2006-10-06 | 2008-04-17 | The Trustees Of Princeton University | Functional graphene-rubber nanocomposites |
| US20090054581A1 (en) * | 2005-10-14 | 2009-02-26 | The Trustees Of Princeton University | Tire containing thermally exfoliated graphite oxide |
| CN102942743A (en) * | 2012-09-26 | 2013-02-27 | 北京化工大学 | Simple preparation method of graphene sheet nano composite material |
| CN102947372A (en) * | 2010-04-22 | 2013-02-27 | 阿克马法国公司 | Thermoplastic and/or elastomeric composite material containing carbon nanotubes and graphenes |
| US20130197256A1 (en) * | 2012-01-26 | 2013-08-01 | Yi-Shuen Wu | Method for the preparation of graphene |
| CN103642018A (en) * | 2013-11-21 | 2014-03-19 | 金发科技股份有限公司 | Graphene oxide/polyester elastomer composite material and preparation method thereof |
| CN103739971A (en) * | 2014-02-12 | 2014-04-23 | 山东科技大学 | Modified graphene nylon/chlorinated isobutylene isoprene rubber (CIIR) thermoplastic elastomer |
| CN105086425A (en) * | 2015-09-17 | 2015-11-25 | 福州大学 | Stacked functionalized graphene nanoribbons/TPU composite material and preparation thereof |
-
2016
- 2016-05-19 CN CN201610333948.8A patent/CN105949728A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090054581A1 (en) * | 2005-10-14 | 2009-02-26 | The Trustees Of Princeton University | Tire containing thermally exfoliated graphite oxide |
| WO2008045778A1 (en) * | 2006-10-06 | 2008-04-17 | The Trustees Of Princeton University | Functional graphene-rubber nanocomposites |
| CN102947372A (en) * | 2010-04-22 | 2013-02-27 | 阿克马法国公司 | Thermoplastic and/or elastomeric composite material containing carbon nanotubes and graphenes |
| US20130197256A1 (en) * | 2012-01-26 | 2013-08-01 | Yi-Shuen Wu | Method for the preparation of graphene |
| CN102942743A (en) * | 2012-09-26 | 2013-02-27 | 北京化工大学 | Simple preparation method of graphene sheet nano composite material |
| CN103642018A (en) * | 2013-11-21 | 2014-03-19 | 金发科技股份有限公司 | Graphene oxide/polyester elastomer composite material and preparation method thereof |
| CN103739971A (en) * | 2014-02-12 | 2014-04-23 | 山东科技大学 | Modified graphene nylon/chlorinated isobutylene isoprene rubber (CIIR) thermoplastic elastomer |
| CN105086425A (en) * | 2015-09-17 | 2015-11-25 | 福州大学 | Stacked functionalized graphene nanoribbons/TPU composite material and preparation thereof |
Non-Patent Citations (1)
| Title |
|---|
| LIYAN MA等: "Functionalized graphene/thermoplastic polyester elastomer nanocomposites by reactive extrusion-based materbatch: preparation and properties reinorcement", 《POLYMERS FOR ADVANCED TECHNOLOGIES》 * |
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