CN104817751B - Method for improving wear resistance and strength of ultrahigh-molecular-weight polyethylene - Google Patents
Method for improving wear resistance and strength of ultrahigh-molecular-weight polyethylene Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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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- C08L2207/00—Properties characterising the ingredient of the composition
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- C08L2207/068—Ultra high molecular weight polyethylene
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Abstract
The invention belongs to polymer composite materials and preparation technology of polymer composite materials and particularly relates to a preparation method of ultrahigh-molecular-weight polyethylene. For solving the shortcomings of low surface hardness, poor abrasion-resistant capability, low strength, poor high-temperature fluidity and the like of the ultrahigh-molecular-weight polyethylene (UHMWPE), the method comprises preparing and adding a compatilizer and modifying materials through a carbon nano tube and silicon dioxide to obtain the performance-optimized UHMWPE. According to the technical scheme, the compatilizer PE-b-M is prepared through ATRP (atom transfer radical polymerization), wherein M is silane coupling agent; the carbon nano tube, the silicon dioxide, the PE-b-M and UHMWPE are heated and uniformly mixed in a certain proportion to hydrolyze and bond the silane coupling agent and the carbon nano tube; the modified UHMWPE is high in compatibility and various properties of the modified UHMWPE can be enhanced.
Description
Technical field
The invention belongs to polymer composites and its technology of preparing, more particularly to a kind of high-performance superhigh molecular weight polyethylene
The preparation method of alkene.
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) is a kind of linear polymer, and molecular weight is crystallized generally 100～5,000,000
Degree 65%～85%, 0.92～0.96g/cm of density3.Compared with other polymers material, the advantage of UHMWPE is that it rubs
Wipe coefficient little, abrasion are low, and chemical proofing is excellent, impact resistance, resistance to pressure etc..These good characteristics have UHMWPE materials
Highly important practical value.Wherein coefficient of friction is little, wear away low, anti-stress cracking performance most attaches most importance in UHMWPE applications
Will.These premium properties make it be widely used in the neck such as coal, military affairs, physical culture, building, medical treatment, chemical industry, weaving, papermaking, agricultural
Domain.
Because ultra-high molecular weight polyethylene strand is very long and mutually tangles, temperature flowing extreme difference, to hot shearing pole
It is insensitive, it is susceptible to shear fracture or generation signs of degradation of being heated.In addition, its wear-resistant grain wear resistance is poor, intensity is low lacking
Point, in order to overcome these defects of UHMWPE, needs to be modified its physical and mechanical properties and processing characteristics.Its method of modifying
It is divided into chemical modification and physical modification.Wherein, physical modification includes addition filler with reinforcing material various aspects of performance, addible
Material has glass microballoon, glass fibre, mica, talcum powder, silica, alundum (Al2O3), carbon black, CNT etc..
Since CNT finds from Japanese Scientists, its unique structure and physicochemical properties are by the extensive of people
Concern, becomes one of focus of research in nearly more than ten years nanometer material science.CNT not only has general nano-particle
Quantum effect, but also with specific surface area is big, high mechanical strength, electrical conductivity it is high, it is heat-resist the features such as so as to show spy
Different mechanics, physics, chemical property, is with a wide range of applications in fields such as electronics, communication, chemical industry, Aeronautics and Astronautics.Closely
Nian Lai, research be concentrated mainly on that surface is modified and composite aspect.But due to the relative 'inertia' of carbon nano tube surface, very
Hardly possible is disperseed in the polymer, need to be to its modifying surface.
The content of the invention
The technical problem to be solved is：Overcome current CNT in superhigh molecular weight polyethylene material
The shortcoming of the existing compatibility of addition, bad dispersibility and temperature flowing difference.
To solve this technical problem, the technical solution used in the present invention is：
Compatilizer PE-b-M is prepared using ATRP method (Transfer Radical Polymerization), to ultra-high molecular weight polyethylene material
Add above-mentioned compatilizer PE-b-M, CNT and silica simultaneously in material, the heating in banbury is mixed, and is modified
UHMWPE, while strengthening ultra-high molecular weight polyethylene its wearability is improved.
Technical scheme is concretely comprised the following steps：
(1) preparation of initiator PE-Br：
7.5gPE-OH and 50mL dimethylbenzene is added in there-necked flask, stirs complete to PE-OH at 70 DEG C in oil bath pan
Room temperature (25 DEG C) is naturally cooled to after CL, under then stirring 20mL triethylamines are added thereto to；It is again that the 2- bromos of 7mL is different
Butyryl bromide is dissolved in 20mL diformazans benzo and dropwise drops in above-mentioned there-necked flask in 15min, drips under room temperature (25 DEG C)
Purification after reaction 24h obtains initiator PE-Br,
(2) preparation of compatilizer PE-b-M：
First reaction vessel is vacuumized successively, eliminating water, the deoxygenation of logical nitrogen three times is heated, is added in above-mentioned reaction vessel and is urged
Agent cuprous bromide and complexing agent bipyridyl, and make its mix complexing, and vacuumize, logical nitrogen, then will prepare in step (1)
Initiator PE-Br is dissolved in methyl phenyl ethers anisole, silane coupler M and is dissolved in after methyl alcohol, and above-mentioned reaction vessel is added in the lump, vacuumizes, leads to nitrogen
Gas 1～3 time, reacts 10h at 75 DEG C, compatilizer PE-b-M is obtained after purification,
As preferred：Silane coupler M：PE-Br：Cuprous bromide：The ratio of the amount of the material of bipyridyl is 40：1：1：3, M
Amount can be adjusted according to required molecular weight,
Wherein, silane coupler M is including KH570, KH550, A-171, A-151 etc.,
Above-mentioned raw materials or reagent (silane coupler M, PE-Br, bipyridyl, cuprous bromide, methyl phenyl ethers anisole, methyl alcohol etc.) use front
Complete eliminating water, deoxygenation are needed, need to be vacuumized at 30 DEG C in vacuum drying chamber and be dried 24h, and letting nitrogen in and deoxidizing 30min；
(3) CNT by the compatilizer PE-b-M prepared in step (2), after processing, silica are added to
In UHMWPE, the heating in banbury is mixed, and obtains modified UHMWPE,
Preferably, CNT can select polytype, such as SWCN, multi-walled carbon nano-tubes, titanium dioxide
The Application Range of silicon also includes micron order, nanoscale etc.；Further, using multi-walled carbon nano-tubes and nanometer grade silica,
Wherein, the CNT after process is referred to：CNT is pre-processed using nitration mixture oxidizing process, it is dense in nitration mixture
Sulfuric acid is 3 with red fuming nitric acid (RFNA) volume ratio：1, pretreatment time 5min, nitration mixture process purpose be：Make hydroxyl on CNT band,
The functional groups such as carboxyl,
Total addition of CNT, silica and compatilizer PE-b-M after above-mentioned process is 1%～10%, is entered
One step ground, addition is 3～5%；The mass ratio of three is 10：2：1,
As preferred：Processing temperature in banbury is 190 DEG C, and process time is 5min.
The beneficial effects of the present invention is：In technical scheme, by adopting ATRP
(ATRP) compatilizer PE-b-M is prepared, then by CNT, silica, PE-b-M and ultra-high molecular weight polyethylene by certain ratio
Example heating is mixed, and there are two kinds of materials of PE and silane coupler on compatilizer, and PE is good with the compatibility of ultra-high molecular weight polyethylene；
Silane coupler part in compatilizer combines with CNT hydrolysis, is combined by chemical bond, strengthens interface interaction power,
Not only compatibility is good for modified UHMWPE, and properties are improved.Improving CNT compatibility in the material can be effective
The coefficient of friction of superhigh molecular weight polyethylene material is reduced, wearability and intensity is improved, anti-attrition, wear-resisting, enhanced effect is played.
The crocking resistance and intensity of modified ultra-high molecular weight polyethylene is significantly improved, and coefficient of friction and wear rate are distinguished
It is reduced to 0.2～0.4,0.5～1.5 × 10-9(g/Nm), specific insulation about 1017～1018Ω/cm2, the stretching of material is strong
Degree brings up to 42～50MPa.
Description of the drawings
Fig. 1：Transmission Fourier In situ ATR-FTIR (FTIR-ATR) of the initiator PE-Br prepared in embodiment 1；
Fig. 2：Transmission Fourier In situ ATR-FTIR (FTIR-ATR) of the compatilizer PE-b-M prepared in embodiment 1；
Characterized with transmission Fourier In situ ATR-FTIR (FTIR-ATR), determined PE-OH, PE-Br, PE-b-
The infrared spectrogram of KH570, analyzes the chemical bond change corresponding to its different absworption peak, and with this initiator and compatilizer are proved
Successfully synthesize：
What Fig. 1 and Fig. 2 were represented respectively is the infrared spectrum of PE-Br and PE-b-KH570.Such as Fig. 1, PE-OH is in 3413cm-1
There are the stretching vibration peak of obvious hydroxyl-OH, 2920cm in place-1, 2851cm-1Locate as-CH2- asymmetric, symmetrical stretching vibration
Peak, 724cm-1Locate as-(CH2)nThe rocking vibration peak of-(n >=4), in the infrared of the PE-Br of gained after connecing bromine and processing
Spectrogram has substantially change to be shown as in 3413cm-1The stretching vibration peak of the hydroxyl-OH at place substantially weakens, 1737cm-1Locate as C=O
Stretching vibration peak, work(is may be described as according to this and prepares initiator PE-Br；
Such as Fig. 2, compared with the infrared spectrum of PE-Br in figure, 3413cm-1The stretching vibration peak of the hydroxyl-OH at place substantially increases
By force, this is to hydrolyze the hydroxyl peak for obtaining, 818cm in KH570-1Locate the stretching vibration peak for Si-C, 1087cm for KH570-1Locate be
The stretching vibration peak of Si-O, thus illustrates successfully to synthesize compatilizer PE-b-KH570.
Fig. 3：The nuclear magnetic spectrogram of the initiator PE-Br prepared in embodiment 1；
Fig. 4：The nuclear magnetic spectrogram of the compatilizer PE-b-M prepared in embodiment 1；
Fig. 3 and Fig. 4 are respectively the nuclear magnetic spectrogram of PE-Br and PE-b-KH570.It is-CH at 1.93ppm such as Fig. 33Upper hydrogen
Absworption peak, thus illustrate successfully to synthesize PE-Br.Fig. 4 and Fig. 3 contrasts are understood into that the peak at 1.93ppm disappears, and illustrates PE-
Br initiation KH570 react and generate PE-b-KH570.It is the methyl hydrogen being connected with silicon oxygen bond in KH570 at 3.58ppm
Peak.Peak area at relatively 1.25 and 3.58ppm understands the segment ratio about 2.8 of PE and KH570：1.
Specific embodiment
1. tensile strength
Determined according to GB/T8804.2-2003 thermoplastic plastic pipes tensile property, the tensile strength of test material and disconnected
Split elongation.
2. coefficient of friction
According to ISO 8295-1986 and GB10006-88 plastic sheeting and thin slice measuring friction coefficient method, in load p=
The dynamic friction of test material under the experimental condition of 200N, relative sliding linear velocity v=0.604m/s and fraction time t=120min
Coefficient.
3. wear rate
Using precision balance test wear rate
4. decay resistance analysis
It it is 20 DEG C in temperature using MSH type corrosive wear testing machines, humidity is to be tested under conditions of 60%.
5. electrical property
According to GB1410-2006 adopt 4399B high resistant instrument, temperature be 20 DEG C, humidity be 60% under conditions of surveyed
Examination, test voltage is 500V.
Embodiment 1
(1) preparation of initiator PE-Br：
By 7.5gPE-OH (UNILIN350, technical grade Y0201, hydroxyl value 127；3 lis of handkerchiefs of viscosity (149 DEG C)) and 50mL bis-
Toluene is added in there-necked flask, to stir to PE-OH at 70 DEG C in oil bath pan and naturally cool to room temperature (25 after being completely dissolved
DEG C), it is added thereto to 20mL triethylamines under then stirring；Again 7mL acylbromides are dissolved in into 20mL diformazan benzos dropwise to drip in 15min
Add in above-mentioned there-necked flask, drip under room temperature (25 DEG C) react 24h after purification obtain initiator PE-Br (transmission Fourier
As shown in Figure 1, nuclear magnetic spectrogram is as shown in Figure 3 for leaf In situ ATR-FTIR (FTIR-ATR)),
(2) preparation of compatilizer PE-b-M：
First reaction vessel is vacuumized successively, eliminating water, the deoxygenation of logical nitrogen three times is heated, is added in above-mentioned reaction vessel and is urged
Agent cuprous bromide and complexing agent bipyridyl, and make its mix complexing, and vacuumize, logical nitrogen, then will prepare in step (1)
Initiator PE-Br is dissolved in methyl phenyl ethers anisole, silane coupler M (KH570) and is dissolved in after methyl alcohol (wherein, silane coupler M：PE-Br：Bromine
Change cuprous：The ratio of the amount of the material of bipyridyl is 40：1：1：3), above-mentioned reaction vessel is added in the lump, vacuumize, logical nitrogen 2 times,
10h is reacted at 75 DEG C, compatilizer PE-b-M (transmission Fourier In situ ATR-FTIR (FTIR-ATR) such as accompanying drawing are obtained after purification
Shown in 2, nuclear magnetic spectrogram is as shown in Figure 4),
(3) compatilizer PE-b-KH570, the nanoscale titanium dioxide prepared in ultra-high molecular weight polyethylene 40g, step (2) is taken
The addition of the multi-walled carbon nano-tubes after silicon, process is respectively 0.2g, 0.4g, 0.2g, and the processing temperature in banbury is 190
DEG C, process time 5min, heating is uniformly mixed so as to obtain modified UHMWPE.
Comparative example 1
Unmodified ultra-high molecular weight polyethylene is selected as comparative example 1.
Comparative example 2
Compared with Example 1, selection does not add compatilizer, CNT and the modified superelevation of silica addition identical
Molecular weight polyethylene is used as comparative example 2, and banbury processing temperature is identical with process time.
Comparative example 3
Compared with Example 1, change banburying machining time for 3min, 7min, 9min, compare material properties.
Comparative example 4
Compared with Example 1, the constant rate of each added material, it is 2%, 4%, 8%, 10% to change total addition,
Compare material properties.
Performance evaluation
In order to measure the properties of the material prepared according to embodiment 1 and comparative example 1～5, carry out as follows
Experiment：
(1) test of tensile strength and elongation at break
(2) coefficient of friction and wear rate are tested
(3) decay resistance analysis
(4) Electrical Analysis
For the modified ultra-high molecular weight polyethylene in embodiment 1, its tensile strength is 45MPa, and elongation at break is
350%, coefficient of friction 0.36, wear rate is 1.2 × 10-9(g/Nm), Erosion-corrosion wear rate is 30 × 10-3/ m, volume electricity
Resistance rate is 1017Ω/cm2。
For the pure ultra-high molecular mass polyethylene in comparative example 1 is tested, its tensile strength be 30MPa, extension at break
Rate is 200%, coefficient of friction 0.45, and wear rate is 2.5 × 10-9(g/Nm), Erosion-corrosion wear rate is 42 × 10-3/ m, body
Product resistivity is 1019Ω/cm2.Modified material various aspects of performance has reinforcement, and shows as more resistant, intensity increase, resists
Electrostatic efficiency is good.
Material modified for comparative example 2, its tensile strength is 35MPa, and elongation at break is 180%, coefficient of friction
0.40, wear rate is 1.8 × 10-9(g/Nm), Erosion-corrosion wear rate is 33 × 10-3/ m, specific insulation is 1017Ω/
cm2.Although compared with pure ultra-high molecular mass polyethylene intensity increase, elongation at break show as decline this explanation filler with it is pure
The compatibility of ultra-high molecular weight polyethylene is bad.
It is as shown in table 1 for the performance of the material obtained by the different process times of comparative example 3.With the increase of process time,
It is little to the entire effect of material, and be conducive to filler to be well mixed wherein, but overlong time may result in material aging
Degrade, therefore process time may be selected in 5min or so：
Impact of the different process times of table 1 to material modified performance
| Sample | 1 | 2 | 3 | 4 |
| Process time/min | 3 | 5 | 7 | 9 |
| Tensile strength/MPa | 43 | 45 | 46 | 43 |
| Elongation at break/% | 270 | 350 | 330 | 330 |
| Coefficient of friction | 0.41 | 0.36 | 0.35 | 0.33 |
| Wear rate/× 10-9g(N·m)-1 | 2.0 | 1.2 | 1.3 | 1.2 |
| Erosion-corrosion wear rate/× 10-3m | 40 | 30 | 29 | 32 |
| Specific insulation/Ω cm-2 | 5.8×1017 | 2.6×1017 | 2.1×10-3 | 3.0×10-3 |
For the constant rate of each added material of comparative example 4, increase addition 2%, 4%, 8%, 10%, it is material modified each
Item performance is as shown in table 2.With the continuous improvement of addition, tensile strength is presented the trend of first increases and then decreases, and this explanation is worked as
When addition increases to 10%, the performance of material itself has excessively been affected because of addition, cause intensity to drop to originally
30MPa, and elongation at break is also lower than pure material, and this also illustrates that addition increases filler and pure ultra-high molecular mass polyethylene
Between compatibility poor.To sum up, preferable addition is 5%.
Impact of the Different adding amount of table 2 to material modified performance
| Sample | 1 | 2 | 3 | 4 | 5 |
| Addition/% | 2 | 4 | 5 | 8 | 10 |
| Tensile strength/MPa | 35 | 42 | 45 | 44 | 30 |
| Elongation at break/% | 250 | 290 | 350 | 300 | 160 |
| Coefficient of friction | 0.43 | 0.39 | 0.36 | 0.35 | 0.32 |
| Wear rate × 10-9/g(N·m)-1 | 2.2 | 1.4 | 1.2 | 1.0 | 1.0 |
| Erosion-corrosion wear rate/× 10-3m | 41 | 37 | 30 | 29 | 29 |
| Specific insulation/Ω cm-2 | 1.1×1018 | 3.4×1017 | 2.6×1017 | 1.3×1017 | 8.5×1016 |
Industrial applicability
As described above, the compatilizer for preparing can be effectively improved CNT and silica in ultra-high molecular weight polyethylene
Central compatibility, and it is easy to process.Material modified various aspects of performance has lifting, with intensity height, rub resistance, anti-quiet
The premium properties such as electricity.
Claims (7)
1. a kind of preparation method of high-performance ultra-high molecular weight polyethylene, it is characterised in that：The preparation method is, using atom
Transferring free-radical polymerization method prepares compatilizer PE-b-M, and above-mentioned compatilizer is added simultaneously in superhigh molecular weight polyethylene material
PE-b-M, CNT and silica, the heating in banbury is mixed, and obtains modified UHMWPE；
The preparation method is concretely comprised the following steps,
(1) preparation of initiator PE-Br
7.5gPE-OH and 50mL dimethylbenzene is added in there-necked flask, stirs completely molten to PE-OH at 70 DEG C in oil bath pan
25 DEG C of room temperature is naturally cooled to after solution, under then stirring 20mL triethylamines are added thereto to；Again 7mL acylbromides are dissolved in into 20mL diformazans
Benzo is dropwise dropped in above-mentioned there-necked flask in 15min, is dripped to react to be purified after 24h at 25 DEG C of room temperature and is caused
Agent PE-Br；
(2) preparation of compatilizer PE-b-M
First reaction vessel is vacuumized successively, eliminating water, the deoxygenation of logical nitrogen three times is heated, in above-mentioned reaction vessel catalyst is added
Cuprous bromide and complexing agent bipyridyl, and make it mix complexing, and vacuumize, lead to nitrogen, then will the middle initiation for preparing of step (1)
Agent PE-Br is dissolved in methyl phenyl ethers anisole, silane coupler M and is dissolved in after methyl alcohol, and above-mentioned reaction vessel is added in the lump, vacuumize, logical nitrogen 1～
3 times, 10h is reacted at 75 DEG C, compatilizer PE-b-M is obtained after purification；
(3) CNT by the compatilizer PE-b-M prepared in step (2), after processing, silica are added in UHMWPE,
The heating in banbury is mixed, and obtains modified UHMWPE,
CNT after described process is referred to, CNT is pre-processed using nitration mixture oxidizing process, in the nitration mixture
The concentrated sulfuric acid is 3 with red fuming nitric acid (RFNA) volume ratio：1, the pretreatment time is 5min.
2. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (2)
Described silane coupler M：PE-Br：Cuprous bromide：The ratio of the amount of the material of bipyridyl is 40：1：1：3.
3. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (2)
Described silane coupler M is KH570, KH550, A-171 or A-151.
4. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (3)
Described CNT is SWCN or multi-walled carbon nano-tubes.
5. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (3)
Described silica is micron silica or nanometer grade silica.
6. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (3)
Described compatilizer PE-b-M, process after CNT, the total addition of silica be 1%～10%.
7. the preparation method of high-performance ultra-high molecular weight polyethylene as claimed in claim 1, it is characterised in that：In step (3)
CNT, silica, compatilizer PE-b-M after described process, the mass ratio of three is 1：2：1.
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