CN106046282A - Diatomite modified by polyaryletherketone containing boric m-benzene and reinforced polyether-ether-ketone composite material thereof - Google Patents
Diatomite modified by polyaryletherketone containing boric m-benzene and reinforced polyether-ether-ketone composite material thereof Download PDFInfo
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- CN106046282A CN106046282A CN201610547065.7A CN201610547065A CN106046282A CN 106046282 A CN106046282 A CN 106046282A CN 201610547065 A CN201610547065 A CN 201610547065A CN 106046282 A CN106046282 A CN 106046282A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/02—Condensation polymers of aldehydes or ketones with phenols only of ketones
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K9/02—Ingredients treated with inorganic 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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Abstract
The invention relates to diatomite modified by polyaryletherketone containing boric m-benzene and a reinforced polyether-ether-ketone composite material thereof, and belongs to the technical field of polymer composite materials. Based on the equation that the sum of proportions of all the components is 100%, the diatomite modified by polyaryletherketone containing boric m-benzene is prepared from 94-98 wt% of diatomite treated with acid and the balance a coupling agent of polyaryletherketone containing boric m-benzene. Under the activating temperature, the diatomite is modified with polyaryletherketone containing boric m-benzene, and the composite material is prepared in the mode similar to in situ polymerization; by adding the coupling agent of polyaryletherketone containing boric m-benzene, the interface interaction between the diatomite and the polyether-ether-ketone can be improved, and mechanical properties of the composite material can be further promoted. Plastifying, melting, injecting, mold filling, cooling and forming and demolding are carried out on the obtained composite material particles through a high-temperature injection molding machine to obtain composite material samples in corresponding shapes.
Description
Technical field
The invention belongs to technical field of polymer composite materials, be specifically related to a kind of boronic acid containing isophthalic PAEK modified silicon
Diatomaceous earth and reinforced polyether ether ketone composite thereof.
Background technology
Kieselguhr is mainly formed by the protective layer skeleton long time sedimentation outside diatom, and its chemical composition is the most unformed
SiO2, generally can use SiO2·nH2O represents, its mineralogical composition is protein and mutation thereof.Owing to kieselguhr has hole
Rate is big, adsorptivity is strong, stable chemical performance, light weight, unit weight are little, thermal insulation good, refractive index is low, dispersibility and suspension good, resistance to
Mill property and the feature such as electrical insulating property is good, so being widely used in light industry, chemical industry, the daily life various aspects such as building materials.
Polyether-ether-ketone (PEEK) is a kind of hemicrystalline thermoplastic resin, accounts in the special engineering plastics of commercialization
There is critical role.Along with the continuous progress of science and technology, people are more and more higher to the requirement of material, except requiring that material has
Outside excellent mechanical performance, in addition it is also necessary to there is the performances such as excellent rub resistance, radioprotective, antistatic, the most even need tool
Standby other functions multiple.Therefore, single virgin resin cannot meet and required, and prepares polyether-ether-ketone as required and is combined
Material becomes the most necessary, composite can not only reinforced polyether ether ketone, and the cost of material can be reduced, allow material
It is more widely applied.Polyether-ether-ketone and inorganic filler, fiber, polymer etc. are blended the mechanicalness that can strengthen it to a certain extent
Can and heat resistance, but polyether-ether-ketone is general and the interfacial interaction of filler is less, does not reaches preferable reinforced effects, one
As need to use coupling agent to be modified filling surface strengthening interface compatibility between the two.Conventional coupling agent includes silicon
Alkane coupling agent, stearic acid coupling agent, boric acid ester coupler etc., also have by synthetically prepared oligomer coupling agent.But polyethers ether
Ketone processing temperature is more than 360 DEG C, and above-mentioned coupling agent high temperature easily decomposes, and does not reaches good modified effect.
Chinese patent CN104017325A reports by boric acid PAEK boric acid modification al whisker reinforced polyether ether ketone
Composite, it is achieved that aluminium borate whisker and the enhancing of polyether-ether-ketone interface compatibility, the stretch bending performance of material all obtains
Large increase.There is presently no use boronic acid containing isophthalic PAEK modification infusorial earth and prepare polyether-ether-ketone/composite diatomite material
The report of material.This composite sample has higher intensity, it is possible to as Aero-Space, weaponry, automobile high temperature resistant
Parts or component of machine etc., the most diatomaceous addition can also the most enough reduce the cost of material.
Summary of the invention
First purpose of the present invention is to provide a kind of boronic acid containing isophthalic PAEK modification infusorial earth and preparation method thereof.
The present invention utilizes boronic acid containing isophthalic PAEK coupling agent and the reaction on kieselguhr surface and good with polyether-ether-ketone
The good compatibility, it is achieved reinforced polyether ether ketone and the purpose of kieselguhr interface compatibility.
Boronic acid containing isophthalic PAEK modification infusorial earth of the present invention, is calculated by each component and 100wt%, wherein silicon
The content of diatomaceous earth is 94～98wt%, and remaining is boronic acid containing isophthalic PAEK coupling agent, wherein, boronic acid containing isophthalic PAEK
The structural formula of coupling agent is as shown in (I), and its preparation method is shown in Chinese patent CN104017325A:
Wherein, 2x+y+z=0.15～0.20, t=1-(2x+y=z)；M represents the degree of polymerization, for the integer more than or equal to 1；
And prepared by following steps:
(1) 100g kieselguhr is dissolved in 300～800mL distilled water, then instill 5～9mol/L diluted acid (dilute sulfuric acid,
Dilute hydrochloric acid, dust technology etc.), the pH making reaction system is 1～3, sucking filtration after stirring 1～2 hour；Wash with water and acetone the most respectively
Wash sucking filtration product 3～5 times, remove impurity therein, vacuum, freeze-day with constant temperature 6～12 hours at 80～100 DEG C；
(2) boronic acid containing isophthalic PAEK coupling agent is joined in reaction vessel, add organic solvent (chloroform
Deng), the volume (mL) of organic solvent is 80～150mL with the ratio of the quality (g) of boronic acid containing isophthalic PAEK coupling agent:
1g, stirring makes coupling agent fully dissolve；The kieselguhr weighing step (1) more acid-treated joins in above-mentioned solution, and room temperature stirs
Mixing 6～12 hours post-heating makes organic solvent reflux, and refluxes 2～4 hours, is cooled to room temperature, filtration drying, finally 150～
Activate 8～12 hours at 180 DEG C, by product organic solvent (chloroform etc.) extracting 10～12 hours, under vacuum
80 DEG C～120 DEG C are dried 10～12 hours, obtain boronic acid containing isophthalic PAEK modification infusorial earth.
Second object of the present invention is to provide a kind of boronic acid containing isophthalic PAEK modification infusorial earth to strengthen polyethers ether
Ketone composite and preparation method thereof.
Boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite of the present invention, the base of use
Body resin is polyether-ether-ketone (PEEK), and by the synthesis of in-situ polymerization process, (concrete preparation method is shown in patent of invention " a kind of diatom
Soil/polyether-ether-ketone composite material and preparation method thereof, CN104559048A ", the structural formula of PEEK such as (II), wherein n represents poly-
Right, the typically greater than integer equal to 1.
Reinforcing material is boronic acid containing isophthalic PAEK modification infusorial earth, and diatomaceous main component is SiO2, have good
Good heat stability and chemical stability, good mechanical strength, high elastic modelling quantity, and it is a kind of natural porous material
Material, has more preferable interface compatibility between boronic acid containing isophthalic PAEK modification infusorial earth and polyether-ether-ketone matrix.
Boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite of the present invention is by similar
Prepared by the mode in in-situ polymerization.
(1) weigh diphenyl sulphone (DPS) (3～4 times of the quality sum of 4,4'-difluoro benzophenones and hydroquinone) and join three
In neck flask, after heating is dissolved under logical condition of nitrogen gas, adding 4,4'-difluoro benzophenone 1～1.1 molar part, hydroquinone 1 rubs
That part, K2CO3And Na2CO3Mixed salt catalyst (two material mol ratios 1～1.5:20) 1～1.2 molar part, are eventually adding dimethylbenzene
(dimethylbenzene volume is 1mL:3～4g with the ratio of diphenyl sulphone (DPS) quality), after reaction carries out 7～8 hours, system viscosity increases, then
Adding 4,4'-difluoro benzophenone 0.01～0.015 molar part, after end-blocking, addition boronic acid containing isophthalic PAEK is coupling agent modified
Kieselguhr (20%～the 25% of the quality sum of 4,4'-difluoro benzophenones and hydroquinone), in-situ polymerization is obtained
Raw material washing is dried, and obtains boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite；Modification infusorial earth
Add after polymerization reaches certain viscosity and blocks, the coming off of coupling agent above the kieselguhr of modification can be avoided as far as possible；
(2) the composite powder that step (1) in-situ polymerization obtains is joined in double screw extruder 360～390
Melt extrude under the conditions of DEG C, after cooling, be cut into a length of 4～6mm, a diameter of 2～the cylinder of 4mm by hobboing cutter pelleter again
Shape granule, i.e. obtains the reinforced polyether ether ketone composite pellet of boronic acid containing PAEK modification infusorial earth of the present invention.
Further, the boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite wood according to said method prepared
In material, calculating by each component and 100wt%, the content of polyether-ether-ketone (structure formula (II)) is 74～94.8wt%, and remaining is for containing
The kieselguhr that boric acid isophthalic PAEK is coupling agent modified；The content of boronic acid containing isophthalic PAEK (structure formula (I)) be 0.2～
1.0wt%, the diatomaceous content after acid treatment is 5～25wt%.
The present invention is to use boronic acid containing isophthalic PAEK coupling agent to be modified kieselguhr under activation temperature, then profit
Preparing composite by the mode being similar to in-situ polymerization, the addition of boronic acid containing isophthalic PAEK coupling agent can improve silicon
Interfacial interaction between diatomaceous earth and polyether-ether-ketone, makes the mechanical property of composite be promoted further.Gained is multiple
Condensation material pellet is by obtaining the compound of respective shapes after high-temperature injection molding machine plastifying fusion, injection, mold filling, cooling molding, the demoulding
Material sample.
Accompanying drawing explanation
Fig. 1 is the boronic acid containing isophthalic PAEK coupling agent described in embodiment 11H-NMR spectrum, it can be seen that polymerization
Each hydrogen atom in thing construction unit is obtained for corresponding ownership；
Fig. 2 is the DSC curve of the boronic acid containing isophthalic PAEK coupling agent described in embodiment 1, used in the present invention
The glass transition temperature of boronic acid containing isophthalic PAEK at 144.2 DEG C；
Fig. 3 be unmodified kieselguhr in embodiment 1 (homologous thread D) and boronic acid containing isophthalic PAEK coupling agent modified after
The TGA curve of kieselguhr (homologous thread D-modified), from TGA curve it can be seen that boronic acid containing isophthalic PAEK coupling
There is a lasting weightless process from 170～480 DEG C in the kieselguhr of agent modification, and 170 DEG C start between weightlessness mainly boronic acid containings
Weightlessness after the removing of a small amount of water in benzene PAEK, 320 DEG C of weightlessness mainly phenylboric acids started decompose and cause, 400 DEG C with
After weightless mainly caused by main chain decomposition, meet major part and contain the thermal decomposition process of borane polymers.Can from TGA figure
Go out: the coupling agent modified kieselguhr of boronic acid containing isophthalic PAEK has good heat stability.
Fig. 4 is the coupling agent modified rear diatomaceous stereoscan photograph of boronic acid containing isophthalic PAEK in embodiment 1
(SEM), substantially there is one layer of coating on the kieselguhr surface that as can be seen from the figure boronic acid containing isophthalic PAEK is coupling agent modified,
The diatomaceous pore structure of part there is also coating, illustrate that boronic acid containing isophthalic PAEK coupling agent the most sufficiently connects
It is connected on kieselguhr surface.
Fig. 5 is the surface sweeping electromicroscopic photograph (SEM) of kieselguhr reinforced polyether ether ketone composite in embodiment 2, can from figure
To see kieselguhr smooth surface, stick to above almost without polyether-ether-ketone resin, kieselguhr surface and polyether-ether-ketone are described
Between resin, interface interaction is more weak, needs the addition of coupling agent to go to strengthen its interfacial interaction to improve performance.
Fig. 6 is the surface sweeping of boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite in embodiment 3
Electromicroscopic photograph (SEM), can be clearly visible kieselguhr surface from figure has polyether-ether-ketone resin to adhere to, modified kieselguhr
And having good interaction between polyether-ether-ketone interface, beneficially between kieselguhr and polyether-ether-ketone, the effective of stress transmits, because of
This shows more preferable reinforced effects, and this meets with mechanical experimental results.Further illustrate boronic acid containing isophthalic PAEK
The effect improving matrix with filler interfacial interaction can be played in preparing polyether-ether-ketone/diatomite composite material.
Detailed description of the invention
Being further described the method for the present invention below by specific embodiment, described embodiment is to this
The specific descriptions of bright claim, claim includes but not limited to described embodiment content.
Embodiment 1: the coupling agent modified diatomaceous preparation of boronic acid containing isophthalic PAEK
(1) as a example by boronic acid containing isophthalic PAEK addition 4wt%, weigh 100g kieselguhr, put into 1000mL beaker
In, adding 500mL distilled water, instill the concentrated sulphuric acid of mass fraction 98% with dropper, regulation pH value is 2, stirs 1 hour, sucking filtration；
Then by sucking filtration product respectively with water and washing with acetone 3 times, impurity therein is removed, 80 DEG C of freeze-day with constant temperature of vacuum 8 hours, standby
With；
(2) weigh 4g boronic acid containing isophthalic PAEK coupling agent, add in the 1000mL there-necked flask containing stirrer, add
Enter the chloroform of 500mL, stirring, treat that it is completely dissolved；
(3) weigh and join in above-mentioned solution through the kieselguhr 96g of acid treatment, stirring at normal temperature 8 hours, it is heated to 62 DEG C and returns
Flow 3 hours；
(4) treating that solution is cooled to room temperature, filtration drying, in vacuum drying oven, 180 DEG C of constant temperature activate 12 hours；
(5) step (4) product chloroform is extracted 12 hours, vacuum, 100 DEG C be dried after 10 hours and obtain by boracic
The coupling agent modified kieselguhr 100g of isophthalic PAEK is standby in acid.Wherein, the theory of boronic acid containing isophthalic PAEK coupling agent
Addition is 4wt%.
Embodiment 2: the preparation of kieselguhr reinforced polyether ether ketone composite is (with kieselguhr content as 20wt%, the most poly-
As a example by conjunction, hydroquinone addition is 0.5mol)
(1) preparation is applicable to the kieselguhr of in-situ polymerization: weighs 100g kieselguhr, puts in 1000mL beaker, adds
500mL distilled water, instills the concentrated sulphuric acid of mass fraction 98% with dropper, and regulation pH value is 2, stirs 2 hours, sucking filtration；Then will
Sucking filtration product, respectively with water and washing with acetone 3 times, removes impurity therein, and 80 DEG C of freeze-day with constant temperature of vacuum 8 hours are standby；
(2) weigh dilute sulfuric acid to process and kieselguhr 36.12g, the diphenyl sulphone (DPS) 520.32g of drying for standby, by diphenyl sulphone (DPS) and silicon
Diatomaceous earth is added sequentially in reaction unit, logical nitrogen after evacuation, the most alternately 3 times.Remaining inventory: Na2CO3
55.48g, K2CO33.80g, 4,4'-difluoro benzophenone 110.19g, hydroquinone 55.06g, dimethylbenzene 70mL (concrete operations
Step is shown in patent " a kind of kieselguhr/polyether-ether-ketone composite material and preparation method thereof, CN104559048A "), by in-situ polymerization
The raw material washing obtained is dried, and obtains polyether-ether-ketone/diatomite composite material that kieselguhr theoretical content is 20wt%.
(3) being melt extruded by double screw extruder by dried composite powder, extrusion temperature is 370 DEG C, cold
But the cylindrical shape granule of a length of 4～6mm, a diameter of 2～4mm it is cut into after again by hobboing cutter pelleter, then by composite wood
Material pellet by injection machine high-temperature injection become stretching and bending test bars, tensile bars intermediate sizes (batten be one mute
Bell type structure, two ends are thick, and middle thin structure is resulting structure) it is 75 × 5 × 2mm, bend batten a size of 4 × 6 × 55mm,
Test bars is designated as PEEK/D20.
Embodiment 3: the preparation of boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite, to implement
Kieselguhr content modified in example 1 is 20wt%, as a example by polymerization, hydroquinone addition is 0.5mol)
(1) weigh diphenyl sulphone (DPS) 510.32g, join in 3000mL three-neck flask, be passed through under condition of nitrogen gas heating and make it molten
Solve, be subsequently adding Na2CO356.48g, K2CO33.20g, 4,4'-difluoro benzophenone 110.23g (0.505mol), to benzene two
Phenol 55.06g (0.5mol), dimethylbenzene 150mL, after reaction carries out 8 hours, after system viscosity increases, add 4,4'-difluorodiphenyl
Kieselguhr 36.63g (its that the boronic acid containing isophthalic PAEK of embodiment 1 preparation is coupling agent modified is added after ketone 1.1g end-blocking
His operating procedure is shown in patent " a kind of kieselguhr/polyether-ether-ketone composite material and preparation method thereof, CN104559048A "), by former
The raw material washing that position polymerization obtains is dried, and obtains the boronic acid containing isophthalic PAEK modification infusorial earth that theoretical content is 20wt% and increases
Strong polyether-ether-ketone composite material.
(2) dried composite powder is prepared as stretching and crooked test batten according to the method in embodiment 2,
Test bars is designated as g-PEEK/D20.
Table 1: pure polyether-ether-ketone, kieselguhr reinforced polyether ether ketone composite, boronic acid containing isophthalic PAEK modification diatom
The mechanical property of soil reinforced polyether ether ketone composite
Note: D20 be in composite kieselguhr content be 20wt%, g be that the kieselguhr in composite is through boronic acid containing
Isophthalic PAEK is modified.Test instrunment: Japan's Shimadzu AG-1 type electronic universal tester.Test mode and condition: draw
When stretching test, rate of extension is 5mm/min, and three-point bend test speed is 2mm/min, and it is thick that flexural deformation size is usually batten
1.5 times of degree.After test terminates, computer testing software can provide the stress-strain diagram of sample automatically, according to input
Batten size, computer can provide relevant intensity, modulus and fault growth rate.Often organize sample during test at least to need to obtain 5
Individual panel data, calculates meansigma methods and obtains end product.
As shown in table 1, kieselguhr reinforced polyether ether ketone composite, its stretching, bending strength and modulus have and substantially carry
Height, fault growth rate reduces.And through the modified kieselguhr reinforced polyether ether ketone composite of boronic acid containing isophthalic PAEK
Stretching, bending strength and modulus have further raising, hence it is evident that higher than answering of non-modified kieselguhr reinforced polyether ether ketone
Condensation material.
Claims (7)
1. a boronic acid containing isophthalic PAEK modification infusorial earth, it is characterised in that: calculate, wherein by each component and 100wt%
Diatomaceous content is 94～98wt%, and remaining is the boronic acid containing isophthalic PAEK coupling agent that structural formula is as follows,
Wherein, 2x+y+z=0.15～0.20, t=1-(2x+y=z)；M represents the degree of polymerization, for the integer more than or equal to 1；
And this boronic acid containing isophthalic PAEK modification infusorial earth is prepared by following steps,
(1) 100g kieselguhr is dissolved in 300～800mL distilled water, then instills in the diluted acid of 5～9mol/L, make reactant
The pH of system is 1～3, sucking filtration after stirring 1～2 hour；The most respectively with water and washing with acetone sucking filtration product 3～5 times, remove wherein
Impurity, vacuum, freeze-day with constant temperature 6～12 hours at 80～100 DEG C；
(2) boronic acid containing isophthalic PAEK coupling agent is joined in reaction vessel, add organic solvent, the body of organic solvent
The ratio of the long-pending quality with boronic acid containing isophthalic PAEK coupling agent is 80～150mL:1g, and stirring makes coupling agent fully dissolve；
Weighing the acid-treated kieselguhr of step (1) again and join in above-mentioned solution, stirring at normal temperature 6～12 hours post-heating make organic molten
Agent refluxes, and refluxes 2～4 hours, is cooled to room temperature, filtration drying, finally activates 8～12 hours at 150～180 DEG C, will produce
Thing organic solvent extracts 10～12 hours, and 80 DEG C～120 DEG C are dried 10～12 hours under vacuum, obtain between boronic acid containing
Benzene PAEK modification infusorial earth.
2. a kind of boronic acid containing isophthalic PAEK modification infusorial earth as claimed in claim 1, it is characterised in that: diluted acid is dilute sulfur
Acid, dilute hydrochloric acid or dust technology.
3. a kind of boronic acid containing isophthalic PAEK modification infusorial earth as claimed in claim 1, it is characterised in that: organic solvent is
Chloroform.
4. a boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite, it is characterised in that: by each group
Dividing and 100wt% calculates, the content of the polyether-ether-ketone that structural formula is as follows is 74～94.8wt%, and remaining is claim 1
～the boronic acid containing coupling agent modified kieselguhr of isophthalic PAEK that 3 described in any one,
N represents the degree of polymerization, for the integer more than or equal to 1；
And this composite is prepared by following steps,
(1) weigh diphenyl sulphone (DPS) and join in three-neck flask, after heating is dissolved under logical condition of nitrogen gas, add 4,4'-difluorodiphenyl first
Ketone 1～1.1 molar part, hydroquinone 1 molar part, K2CO3And Na2CO3Mixed salt catalyst 1～1.2 molar part, is eventually adding two
Toluene, after reaction carries out 7～8 hours, system viscosity increases, and adds 4,4'-difluoro benzophenone 0.01～0.015 mole
Part, adding the boronic acid containing coupling agent modified kieselguhr of isophthalic PAEK after end-blocking, the raw material obtained by in-situ polymerization washing is dried,
Obtain boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite；
(2) the composite powder that step (1) in-situ polymerization obtains is joined in double screw extruder at 360～390 DEG C of bars
Melt extrude under part, after cooling, be cut into a length of 4～6mm, a diameter of 2～the cylindrical shape of 4mm by hobboing cutter pelleter again
Grain, i.e. obtains the reinforced polyether ether ketone composite pellet of boronic acid containing PAEK modification infusorial earth.
5. a kind of boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite as claimed in claim 4,
It is characterized in that: the quality consumption of diphenyl sulphone (DPS) is 4,3～4 times of the quality sum of 4'-difluoro benzophenone and hydroquinone, two
Volume of toluene is 1mL:3～4g with the ratio of diphenyl sulphone (DPS) quality.
6. a kind of boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite as claimed in claim 4,
It is characterized in that: K2CO3And Na2CO3Mol ratio be 1～1.5:20.
7. a kind of boronic acid containing isophthalic PAEK modification infusorial earth reinforced polyether ether ketone composite as claimed in claim 4,
It is characterized in that: the coupling agent modified kieselguhr quality consumption of boronic acid containing isophthalic PAEK is 4,4'-difluoro benzophenone with
The 20%～25% of the quality sum of hydroquinone.
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|---|---|---|---|
| CN201610547065.7A CN106046282A (en) | 2016-07-13 | 2016-07-13 | Diatomite modified by polyaryletherketone containing boric m-benzene and reinforced polyether-ether-ketone composite material thereof |
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| CN201610547065.7A CN106046282A (en) | 2016-07-13 | 2016-07-13 | Diatomite modified by polyaryletherketone containing boric m-benzene and reinforced polyether-ether-ketone composite material thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929864A (en) * | 2021-11-20 | 2022-01-14 | 扬州工业职业技术学院 | Flame-retardant heat-preservation polyurethane material |
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| CN103626994A (en) * | 2013-11-16 | 2014-03-12 | 吉林大学 | Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof |
| CN104017325A (en) * | 2014-06-10 | 2014-09-03 | 吉林大学 | Polyaryletherketone borate-modified aluminum borate crystal whisker reinforced polyether-ether-ketone composite material and preparation method thereof |
| CN104559048A (en) * | 2015-01-28 | 2015-04-29 | 吉林大学 | Diatomite/polyether-ether-ketone composite material and preparation method thereof |
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| CN103626994A (en) * | 2013-11-16 | 2014-03-12 | 吉林大学 | Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof |
| CN104017325A (en) * | 2014-06-10 | 2014-09-03 | 吉林大学 | Polyaryletherketone borate-modified aluminum borate crystal whisker reinforced polyether-ether-ketone composite material and preparation method thereof |
| CN104559048A (en) * | 2015-01-28 | 2015-04-29 | 吉林大学 | Diatomite/polyether-ether-ketone composite material and preparation method thereof |
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| CN113929864A (en) * | 2021-11-20 | 2022-01-14 | 扬州工业职业技术学院 | Flame-retardant heat-preservation polyurethane material |
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Application publication date: 20161026 |