CN109096692A - A kind of antistatic PEEK resin material and preparation method thereof - Google Patents
A kind of antistatic PEEK resin material and preparation method thereof Download PDFInfo
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- CN109096692A CN109096692A CN201810537808.1A CN201810537808A CN109096692A CN 109096692 A CN109096692 A CN 109096692A CN 201810537808 A CN201810537808 A CN 201810537808A CN 109096692 A CN109096692 A CN 109096692A
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- carbon black
- benzocyclobutene
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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
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
Abstract
The invention discloses a kind of antistatic PEEK resin materials and preparation method thereof.According to the mass fraction, antistatic PEEK resin material is made of 70-90 parts of PEEK and 10-30 parts of modified carbon blacks, and modified carbon black is surface-treated through N- (benzocyclobutene -4- base) maleimide (or and N-phenylmaleimide) by carbon black and is obtained.The application is surface-treated carbon black using N- (benzocyclobutene -4- base) maleimide (or and N-phenylmaleimide), to improve the lipophilicity and dispersibility of carbon black, carbon black is dispersed in PEEK, PEEK resin material has excellent elongation at break and surface resistivity；Since benzocyclobutane alkenyl group has excellent thermal stability, the decomposition temperature of modified carbon black reaches 450 DEG C or more, will not thermally decompose under 370-390 DEG C of PEEK processing temperature.
Description
Technical field
The invention belongs to resin material fields, and in particular to a kind of antistatic PEEK resin material and preparation method thereof.
Background technique
Polyether-ether-ketone, English name polyetheretherketone (abbreviation PEEK), it is to contain chain in molecular backbone
The Linear aromatic macromolecular compound of section.PEEK resin is a kind of special engineering plastics haveing excellent performance, with other extraordinary works
Engineering plastics, which are compared, has more significant advantages, for example, 260 DEG C of resistance to positive high temperature, mechanical performance is excellent, and self-lubrication is good, chemically-resistant
Product corrosion, fire-retardant, peel resistance, wearability, anti-radiation intolerant to strong nitric acid, the concentrated sulfuric acid, superpower mechanical performance, PEEK are navigating
It is used widely in the fields such as empty space flight, automobile manufacture, electric, medical and food processing.
PEEK resin material has fabulous electrical insulating property, has antistatic to meet special dimension to polyether-ether-ketone product
PEEK antistatic bar or plate are developed in the requirement of performance.Traditional handicraft generallys use the conductive materials such as carbon fiber or carbon black
Be blended with PEEK material and prepare antistatic PEEK material, but due to the agglomeration of carbon fiber, directly by carbon fiber or carbon black with
PEEK blending will lead to integral material degraded toughness, and reuniting causes carbon fiber to be evenly distributed in PEEK matrix, final to go back
The sheet resistance for influencing whether integral material reduces its antistatic performance.
First being modified to carbon fibre materials such as carbon blacks before being blended with PEEK is the breach to solve the above problems.
Such as application No. is the Chinese patent applications of CN 201510738521.1 to disclose a kind of antistatic PEEK resin material, this resists quiet
Electric PEEK resin material is made of 68-84 parts of PEEK, 15-30 parts of chopped carbon fibers, 1-2 parts of carbon nanotubes, wherein carbon nanotube
It is surface-treated by sulfonation PEEK, the sulfonation degree of sulfonation PEEK is 70-80, and chopped carbon fiber is then through surface oxidation treatment (500
It is handled 6-8 hours at DEG C).
There is also following defects for above-mentioned PEEK resin material: (1) carbon nanotube is modified using high sulfonation PEEK, however
The thermal stability of high sulfonation PEEK is lower, and the weight loss at 400 DEG C can reach 35%, and the processing temperature of PEEK is usually
Between 370-390 DEG C, when carrying out PEEK processing, high sulfonation PEEK can be decomposed, it is made to lose work to the surface modification of carbon black
With；(2) chopped carbon fiber needs handle 6-8 hours realization surfaces at 500 DEG C and are modified, and modified condition is more harsh, to equipment
It is more demanding；(3) elongation at break of the PEEK resin material finally obtained only has 8.4-11.7%, and toughness of material is lower to be shown
The agglomeration traits of carbon fiber are solved there is no thorough, and the distribution of carbon fiber is still uneven in material.
Summary of the invention
Present invention purpose is to provide that a kind of carbon fiber is evenly distributed, reunites there is no carbon fiber and thermal stability is high
Antistatic PEEK resin material.
Foregoing invention purpose is not implemented, the technical solution of the application is as follows:
A kind of antistatic PEEK resin material, according to the mass fraction, by 70-90 parts of PEEK and 10-30 parts of modified carbon black groups
At the modified carbon black is handled through N- (benzocyclobutene -4- base) maleimide surface by carbon black and obtained.
The application is surface-treated carbon black using N- (benzocyclobutene -4- base) maleimide, N- (benzocyclobutane
Alkene -4- base) maleimide can be improved the lipophilicity and dispersibility of carbon black, so that carbon black can be dispersed in PEEK,
It is not in carbon black aggregate, so that antistatic PEEK resin material has excellent elongation at break and antistatic property.
Also, benzocyclobutane alkenyl group and acid imide five-membered ring that N- (benzocyclobutene -4- base) maleimide has
Structure all has excellent thermal stability, point of the modified carbon black after N- (benzocyclobutene -4- base) is Maleimide-modified
Solution temperature reaches 450 DEG C or more, so that modified carbon black still has excellent under 370-390 DEG C of PEEK processing temperature
Thermal stability will not thermally decompose.
Moreover, N- (benzocyclobutene -4- base) maleimide also has good mechanics and electric property, can
Further increase the antistatic property and tensile strength of the antistatic PEEK resin material of the application.
Preferably, the modified carbon black is by carbon black through N- (benzocyclobutene -4- base) maleimide and N- phenyl
Maleimide surface processing obtains.
Carbon black is modified simultaneously using N-phenylmaleimide and N- (benzocyclobutene -4- base) maleimide
Afterwards, the performance of PEEK bar also can be further improved, this may be because of N-phenylmaleimide and N- (benzocyclobutene-
4- yl) maleimide reacts what the polymer to be formed was formed after being grafted or being covered on carbon blacksurface by Diels-Alder
Particle intensity is bigger, and dispersibility further increases, and then PEEK bar can obtain good elongation at break and sheet resistance
Rate.
Preferably, according to the mass fraction, the antistatic PEEK resin material is by 80-85 parts PEEK and 15-20 parts
Modified carbon black composition.
Present invention also provides the preparation method of the antistatic PEEK resin material described in one kind, which is successively wrapped
Include following steps:
(1) modified carbon black is prepared；
This application provides the preparation methods of two kinds of modified carbon blacks: A and B, and wherein A method includes: by carbon black and N- (benzo
Cyclobutane -4- base) maleimide mixing, Diels-Alder reaction is carried out, is obtained through N- (benzocyclobutene -4- base) Malaysia
The modified carbon black of acid imide surface treatment；
B method includes: to mix carbon black, N- (benzocyclobutene -4- base) maleimide and N-phenylmaleimide,
Diels-Alder reaction is carried out, is obtained through N- (benzocyclobutene -4- base) maleimide and N-phenylmaleimide surface
The modified carbon black of processing.
When carrying out carbon black modified using A method, not only N- (benzocyclobutene -4- base) maleimide meeting and carbon blacksurface
Conjugated diene structure occur Diels-Alder reaction, make carbon blacksurface graft N-(benzocyclobutene -4- base) maleimide
(hexatomic ring is aggregated by acid imide five-membered ring and conjugated diene and realizes grafting), improve the dispersibility of carbon black, lipophilicity and
Thermal stability；And Diels-Alder reaction (N- can also occur between N- (benzocyclobutene -4- base) maleimide monomer
The benzocyclobutene of (benzocyclobutene -4- base) maleimide monomer open loop and another N- (benzocyclobutene -4- at high heat
Base) the acid imide five-membered ring on maleimide aggregates into hexatomic ring), thus N- (benzocyclobutene -4- base) maleimide
Carbon black particle can be polymerized to chain or botryoidalis or netted condensate, contain multiple " N- (benzocyclobutenes-in condensate
4- yl) maleimide+carbon black+N- (benzocyclobutene -4- base) maleimide " repetitive unit, leads between two repetitive units
It crosses respective N- (benzocyclobutene -4- base) maleimide and realizes connection；And due to N- (benzocyclobutene -4- base) Malaysia
Imido acid imide five-membered ring has space steric effect, so that polymerization long-chain will not occur to turn round and reunite；Same carbon black
It can also be grafted more N- (benzocyclobutene -4- base) maleimide on particle, make condensate in botryoidalis or netted；This
Allowing for modified carbon black has high structural, survivable spatial network is formed, due to N- (benzocyclobutene -4- base)
Maleimide itself has good mechanics and electric property, therefore is capable of forming in the spatial network and leads without several chain types
Electric structure assigns the excellent electric conductivity of PEEK.
Similarly, when carrying out carbon black modified using B method, not only carbon blacksurface being capable of graft N-(benzocyclobutene -4-
Base) maleimide and N-phenylmaleimide, and between N- (benzocyclobutene -4- base) maleimide monomer, N-
Diels-Alder can occur between maleimide monomer and N-phenylmaleimide monomer for (benzocyclobutene -4- base)
Reaction, this is allowed in the spatial network for the condensate to be formed, chain type conductive structure accumulate more closely, network extent it is higher,
While the dispersibility, lipophilicity and thermal stability for further increasing carbon black, antistatic PEEK resin can be further enhanced
The electric conductivity of material assigns its excellent antistatic property.
Either A method or B method are required to for the carbon black being placed in front of carrying out Diels-Alder reaction
Dry 25h or more, uses after cooling at 100-110 DEG C.Carbon black has certain water imbibition, but is adsorbed on the hydrone on carbon black
It will affect subsequent carbon black and N- (benzocyclobutene -4- base) maleimide or N- (benzocyclobutene -4- base) maleimide
With the reaction of N-phenylmaleimide, influence modified to the surface of carbon black.
When carrying out carbon black modified using A method, the mass ratio of N- (benzocyclobutene -4- base) maleimide and carbon black
For (0.01-30): 100；Preferably, the mass ratio of N- (benzocyclobutene -4- base) maleimide and carbon black is (3-7):
100；It is highly preferred that the mass ratio of N- (benzocyclobutene -4- base) maleimide and carbon black is 6:100；In above-mentioned mixing
Under ratio, N- (benzocyclobutene -4- base) maleimide is best to the thermal stability result for improving carbon black.
When carrying out carbon black modified using B method, N- (benzocyclobutene -4- base) maleimide, N- phenyl Malaysia acyl
The mass ratio of imines and carbon black is (2-4): (2-4): 100.With merely using N- (benzocyclobutene -4- base) maleimide into
The modification of row surface is compared, and carries out table jointly using N- (benzocyclobutene -4- base) maleimide and N-phenylmaleimide
Face is modified, energy while reaching individually modified can achieve the effect that with N- (benzocyclobutene -4- base) maleimide
The dosage for enough reducing N- (benzocyclobutene -4- base) maleimide, is greatly saved carbon black modified cost.
In the preparation method of above-mentioned modified carbon black, the reaction condition of the Diels-Alder reaction are as follows: in 150-
1-7h is reacted at 200 DEG C.Preferably, the reaction condition that Diels-Alder reacts in A method are as follows: react 4-5h at 170 DEG C；B
The reaction condition that Diels-Alder reacts in method are as follows: react 3-4h at 200 DEG C.
(2) modified carbon black and PEEK are mixed by preset parts by weight, dry 4-12h, cooling at 100-200 DEG C；
(3) mixed material after cooling is molded into profile at 370-390 DEG C.
Shooting Technique is molded the profile root of acquisition using conventional in the prior art PEEK Shooting Technique and injection molding machine
According to needing can be bar, plate, sheet material or membrane material.
Compared with prior art, the invention has the benefit that
(1) using N- (benzocyclobutene -4- base), maleimide is surface-treated carbon black to the application, to improve
The lipophilicity and dispersibility of carbon black, enable carbon black to be dispersed in PEEK, are not in carbon black aggregate, so that preventing quiet
Electric PEEK resin material has excellent elongation at break and antistatic property.
(2) there is benzocyclobutane alkenyl group and acyl in N- (benzocyclobutene -4- base) maleimide that the application uses
Imines five-membered ring, the two groups all have excellent thermal stability, Maleimide-modified through N- (benzocyclobutene -4- base)
The decomposition temperature of modified carbon black afterwards reaches 450 DEG C or more, thus under 370-390 DEG C of PEEK processing temperature, Modified Activated Carbon
It is black that still there is excellent thermal stability, it will not thermally decompose；Moreover, N- (benzocyclobutene -4- base) maleimide
Amine also has good mechanics and electric property, can further increase the antistatic of the antistatic PEEK resin material of the application
Performance and tensile strength.
(3) the application substitutes part N- (benzocyclobutene -4- base) maleimide pair using N-phenylmaleimide
After carbon black is modified, the performance of PEEK bar also be can be further improved, this may be because of N-phenylmaleimide and N-
(benzocyclobutene -4- base) maleimide is reacted the polymer to be formed by Diels-Alder and is being grafted or is being covered on carbon black
The particle intensity formed behind surface is bigger, and dispersibility further increases, and then PEEK bar can obtain good extension at break
Rate and antistatic property.
(4) the application is modified carbon black using dry method, and wet-process modified postprocessing working procedures, simple process is omitted.
Specific embodiment
Specific embodiment is set forth below, and further details of the technical solution of the present invention.
PEEK, carbon black, N- (benzocyclobutene -4- base) maleimide and N- phenyl horse as used in the following examples
Carrying out acid imide can be used marketable material, and N- (benzocyclobutene -4- base) maleimide is also referred to document: Tan
L.S.,Arnlod F.E..Resin systems derived from benzocyclobutene-maleimide
Documented method preparation in compounds:US, 4916235 [P] .1990-04-10..Preparation-obtained PEEK bar
Model existsBetween.
Embodiment 1
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:0.01, and is uniformly dispersed in high speed mixer, is transferred in 150 DEG C of reaction kettles after being uniformly dispersed
It carries out Diels-Alder to react 7 hours, obtains modified carbon black.
(2) 70 parts of PEEK and 30 part of modified carbon blacks are taken, uniformly mixed be placed in 100 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 2
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:3, and is uniformly dispersed in high speed mixer, be transferred to after being uniformly dispersed in 170 DEG C of reaction kettles into
Row Diels-Alder reacts 4 hours, obtains modified carbon black.
(2) 80 parts of PEEK and 20 part of modified carbon blacks are taken, uniformly mixed be placed in 150 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 3
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:5, and is uniformly dispersed in high speed mixer, be transferred to after being uniformly dispersed in 170 DEG C of reaction kettles into
Row Diels-Alder reacts 4 hours, obtains modified carbon black.
(2) 80 parts of PEEK and 20 part of modified carbon blacks are taken, uniformly mixed be placed in 150 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 4
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:7, and is uniformly dispersed in high speed mixer, be transferred to after being uniformly dispersed in 170 DEG C of reaction kettles into
Row Diels-Alder reacts 5 hours, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 5
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:15, and is uniformly dispersed in high speed mixer, be transferred to after being uniformly dispersed in 200 DEG C of reaction kettles into
Row Diels-Alder reacts 5 hours, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 6
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine is mixed with the mass ratio of 100:30, and is uniformly dispersed in high speed mixer, be transferred to after being uniformly dispersed in 200 DEG C of reaction kettles into
Row Diels-Alder reacts 7 hours, obtains modified carbon black.
(2) 90 parts of PEEK and 10 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 7
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine, N-phenylmaleimide are uniformly dispersed in high speed mixer with mass ratio 100:2:4 mixing, are turned after being uniformly dispersed
Enter to carry out Diels-Alder reaction 5 hours in 170 DEG C of reaction kettles, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 8
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine, N-phenylmaleimide are uniformly dispersed in high speed mixer with mass ratio 100:3:3 mixing, are turned after being uniformly dispersed
Enter to carry out Diels-Alder reaction 5 hours in 170 DEG C of reaction kettles, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 9
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine, N-phenylmaleimide are uniformly dispersed in high speed mixer with mass ratio 100:4:2 mixing, are turned after being uniformly dispersed
Enter to carry out Diels-Alder reaction 5 hours in 170 DEG C of reaction kettles, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Embodiment 10
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, it is cooling after with N- (benzocyclobutene -4- base) maleimide
Amine, N-phenylmaleimide are uniformly dispersed in high speed mixer with mass ratio 100:4:2 mixing, are turned after being uniformly dispersed
Enter to carry out Diels-Alder reaction 3 hours in 200 DEG C of reaction kettles, obtains modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Comparative example 1
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) 85 parts of PEEK, 15 parts of carbon blacks, 5 parts of lubricants and 5 parts of dispersing agents are taken, is placed in high speed mixer and is uniformly mixed
It is placed in 200 DEG C of baking ovens and removes moisture content, after being completely dried, cooling is spare；
(2) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
Comparative example 2
A kind of preparation method of antistatic PEEK resin material of the present embodiment, comprising the following steps:
(1) modified carbon black is prepared；
Carbon black is placed at 100-110 DEG C dry 25h or more, with N-phenylmaleimide with mass ratio 100 after cooling:
6 mixing, and be uniformly dispersed in high speed mixer, progress Diels-Alder reaction in 200 DEG C of reaction kettles is transferred to after being uniformly dispersed
3 hours, obtain modified carbon black.
(2) 85 parts of PEEK and 15 part of modified carbon blacks are taken, uniformly mixed be placed in 200 DEG C of baking ovens is placed in high speed mixer
Moisture content is removed, after being completely dried, cooling is spare；
(3) mixed material after cooling is transferred in injection molding machine, is molded into bar at 370-390 DEG C.
The PEEK bar of the various embodiments described above preparation is tested for the property, test result is shown in Table 1.
Table 1
| Embodiment | Tensile strength/Mpa | Elongation at break/% | Surface resistivity/Ω |
| Embodiment 1 | 88 | 50% | 8×106 |
| Embodiment 2 | 105 | 68% | 2×106 |
| Embodiment 3 | 117 | 75% | 1.4×106 |
| Embodiment 4 | 109 | 70% | 1.8×106 |
| Embodiment 5 | 94 | 57% | 6×106 |
| Embodiment 6 | 92 | 55% | 6×106 |
| Embodiment 7 | 105 | 72% | 2×106 |
| Embodiment 8 | 108 | 71% | 1.7×106 |
| Embodiment 9 | 112 | 74% | 1.5×106 |
| Embodiment 10 | 119 | 77% | 1×106 |
| Comparative example 1 | 48 | 10% | 4×1010 |
| Comparative example 2 | 60 | 47% | 7×1012 |
As shown in table 1, carbon black is grafted using N- (benzocyclobutene -4- base) maleimide of proper proportion
When modified (embodiment 2- embodiment 4), the tensile strength and elongation at break of the PEEK bar of acquisition are effectively promoted, table
Surface resistivity is down to 1.4 × 106Ω；Although and embodiment 5 and embodiment 6 have good tensile strength but elongation at break phase
To lower, it may be possible to form excessive poly- N-phenylmaleimide when modified and be wrapped in carbon blacksurface, lead to modified carbon black
Toughness is insufficient.
When being modified to carbon black, if being modified (comparative example 2) only with N-phenylmaleimide, acquisition
The properties of PEEK bar are undesirable, but when using N-phenylmaleimide substitution part N- (benzocyclobutene -4-
Base) maleimide is modified (embodiment 7-10), the properties of obtained PEEK bar not only with embodiment 2-4 phase
Closely, and adjust N-phenylmaleimide and N- (benzocyclobutene -4- base) maleimide ratio, the property of PEEK bar
It can also can be further improved, this may be because of N-phenylmaleimide and N- (benzocyclobutene -4- base) maleimide
The polymer to be formed is reacted by Diels-Alder, and chain type conductive structure heap is capable of forming after being grafted or being covered on carbon blacksurface
Product more closely, the higher spatial network of network extent, further enhance the electric conductivity of antistatic PEEK resin material, assign it
Excellent antistatic property.
Claims (10)
1. a kind of antistatic PEEK resin material, which is characterized in that according to the mass fraction, changed by 70-90 parts PEEK and 10-30 parts
Property carbon black composition, the modified carbon black by carbon black through N- (benzocyclobutene -4- base) maleimide surface handle obtain.
2. antistatic PEEK resin material as described in claim 1, which is characterized in that the preparation method of the modified carbon black
Include: to mix carbon black with N- (benzocyclobutene -4- base) maleimide, carry out Diels-Alder reaction, obtains through N-
The modified carbon black of (benzocyclobutene -4- base) maleimide surface processing.
3. antistatic PEEK resin material as described in claim 1, which is characterized in that the modified carbon black is by carbon black through N-
(benzocyclobutene -4- base) maleimide and N-phenylmaleimide surface treatment obtain.
4. antistatic PEEK resin material as described in claim 1, which is characterized in that the preparation method of the modified carbon black
Include: to mix carbon black, N- (benzocyclobutene -4- base) maleimide and N-phenylmaleimide, carries out Diels-
Alder reaction obtains the modification being surface-treated through N- (benzocyclobutene -4- base) maleimide and N-phenylmaleimide
Carbon black.
5. antistatic PEEK resin material as claimed in claim 2 or 4, which is characterized in that carry out Diels-Alder reaction
Before, the carbon black is placed at 100-110 DEG C dry 25h or more, is used after cooling.
6. antistatic PEEK resin material as claimed in claim 2, which is characterized in that N- (benzocyclobutene -4- base) Malaysia
The mass ratio of acid imide and carbon black is (0.01-30): 100.
7. antistatic PEEK resin material as claimed in claim 4, which is characterized in that N- (benzocyclobutene -4- base) Malaysia
The mass ratio of acid imide, N-phenylmaleimide and carbon black is (2-4): (2-4): 100.
8. antistatic PEEK resin material as claimed in claim 2 or 4, which is characterized in that the Diels-Alder reaction
Reaction condition are as follows: react 1-7h at 150-200 DEG C.
9. antistatic PEEK resin material as described in claim 1, which is characterized in that according to the mass fraction, by 80-85 parts
PEEK and 15-20 parts of modified carbon black composition.
10. the preparation method of the antistatic PEEK resin material as described in any one of claim 1-9, which is characterized in that
Successively the following steps are included:
(1) modified carbon black is prepared；
(2) modified carbon black and PEEK are mixed by preset parts by weight, dry 4-12h, cooling at 100-200 DEG C；
(3) mixed material after cooling is molded into profile at 370-390 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230863A (en) * | 2021-11-29 | 2022-03-25 | 安徽大学 | Graphene and carbon black compounded reinforcing heat-conducting filler and application thereof in preparation of high-strength high-elasticity heat-conducting styrene-butadiene rubber composite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150060738A1 (en) * | 2008-06-07 | 2015-03-05 | Hexcel Composites Limited | Conductivity of Resin Materials and Composite Materials |
| CN104987659A (en) * | 2015-08-10 | 2015-10-21 | 广州索润环保科技有限公司 | Heat-resistant antistatic conductive polymer composite material and preparation method therefor and application thereof |
| CN105524412A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic peek resin material and preparation method thereof |
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2018
- 2018-05-30 CN CN201810537808.1A patent/CN109096692B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150060738A1 (en) * | 2008-06-07 | 2015-03-05 | Hexcel Composites Limited | Conductivity of Resin Materials and Composite Materials |
| CN104987659A (en) * | 2015-08-10 | 2015-10-21 | 广州索润环保科技有限公司 | Heat-resistant antistatic conductive polymer composite material and preparation method therefor and application thereof |
| CN105524412A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic peek resin material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230863A (en) * | 2021-11-29 | 2022-03-25 | 安徽大学 | Graphene and carbon black compounded reinforcing heat-conducting filler and application thereof in preparation of high-strength high-elasticity heat-conducting styrene-butadiene rubber composite material |
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