CN106947075B - A kind of poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic method - Google Patents
A kind of poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic method Download PDFInfo
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- CN106947075B CN106947075B CN201710181061.6A CN201710181061A CN106947075B CN 106947075 B CN106947075 B CN 106947075B CN 201710181061 A CN201710181061 A CN 201710181061A CN 106947075 B CN106947075 B CN 106947075B
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
- C08G65/4031—(I) or (II) containing nitrogen
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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
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/46—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing halogen
- C08G2650/48—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing halogen containing fluorine, e.g. perfluropolyethers
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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
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/50—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing nitrogen, e.g. polyetheramines or Jeffamines(r)
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- Organic Insulating Materials (AREA)
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Abstract
The invention discloses a kind of poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic methods, it is with perfluorocyclobutanearyl aryl-ether phenol polymer, hexafluoro bisphenol-a, phenyl-dihalide formonitrile HCN or dihalo para-Phthalonitrile, 4,4 '-difluoro benzophenones are raw material, under catalyst and nitrogen atmosphere, after temperature control reaction twice, drying is precipitated, be filtered, washed and be centrifuged, poly(aryl ether ketone) CABLE MATERIALS resin is obtained.The material effectively improves thermal stability, crystallinity and the dissolubility of polymer, reduce dielectric constant, the dielectric dissipation factor, the rate of signal attenuation of High Speed Transfer frequency band of polymer, the excellent properties for maintaining poly(aryl ether ketone) material make the poly(aryl ether ketone) material while having the advantages that poly (arylene ether nitrile), polyether-ether-ketone and three kinds of materials containing fluorine structure.
Description
Technical field
The present invention relates to a kind of poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic methods, belong to polymeric material field.
Background technique
Poly(aryl ether ketone) is a kind of aromatics thermoplastic special engineering plastic, has good physics and chemical property, thus often
By as CABLE MATERIALS.However, formation homogeneous blend is more difficult between traditional poly aryl ether ketone polymer, preparation process is required more
Complexity, and the auxiliary agent of its addition is more, undoubtedly increases product cost, reduces the reliability of cable.In recent years, around changing
Kind processing performance, improves temperature classification problem, continually develops the such new material haveing excellent performance to meet different requirements.
Such as different functional groups, such as naphthalene nucleus, azepine naphthalene nucleus are introduced in polymerization owner's refining；Also will distort non-co-planar
Phthalazinone, which is introduced into main polymer chain, can improve its dissolubility, while assign its good heat resistance and in master
Different functional groups, such as benzene or trifluoromethyl, the dissolubility and heat resistance of Lai Tigao poly(aryl ether ketone) are introduced on chain.
Wherein, poly (arylene ether nitrile) is a kind of high performance engineering plastics containing cyano side group, has excellent high temperature resistant, corrosion resistant
Erosion, radiation hardness, fire-retardant, balanced physical mechanical property and fabulous dimensional stability.Due to highly polar cyano side group (- CN)
Introducing, on the one hand increase the dipole-dipole effect of molecule interchain, be conducive to obtaining higher heat resistance and machinery is strong
While spending, the adhesive force of reinforced resin matrix；On the other hand, cyano can form as a potential crosslinking points and have more
The network structure of high heat resistance.
In addition, making electric wire made of insulation and sheath material with fluoroplastics (such as polytetrafluoroethylene (PTFE), perfluoroethylene-propylene etc.)
Cable, the oxygen index (OI) of fluoroplastics material are PE plastics more than 3 times, are 1.5 times of PVC plastic；Its combustion heat release amount is only timber
A quarter, be PE plastics 1/7th；The cigarette generated under similarity condition is more much smaller than PVC material；Its combustion product pair
Equipment, the corrosivity of instrument ratio PE, PVC material are low.In addition to this, its dielectric constant, dielectric dissipation factor, High Speed Transfer frequency
The wire and cable of the signal attenuation ratio other materials of band is all small, and physical mechanical property is better than other materials.The present invention is to prepare to contain
There are cyano and a kind of poly(aryl ether ketone) CABLE MATERIALS resin containing fluorine structure, the applicant is by cyano and perfluorocyclobutanearyl aryl-ether structure
It is introduced into poly(aryl ether ketone), thermal stability, crystallinity and the dissolubility of polymer can be effectively improved, reduce polymerization
The dielectric constant of object, dielectric dissipation factor, the rate of signal attenuation of High Speed Transfer frequency band, maintain the excellent of poly(aryl ether ketone) material
Anisotropic energy, makes the poly(aryl ether ketone) material while having the advantages that three kinds of poly (arylene ether nitrile), polyether-ether-ketone and fluorine materials.
Summary of the invention
In order to solve the above problem present in the prior art, the present invention provides a kind of poly(aryl ether ketone) CABLE MATERIALS resin and
The poly(aryl ether ketone) CABLE MATERIALS resin of its synthetic method, this method preparation has good heat resistance and more crosslinking points.
Technical scheme is as follows:
The invention discloses a kind of poly(aryl ether ketone) CABLE MATERIALS resin, structural formulas
It is as follows:
M and n indicates the degree of polymerization, is positive integer.Wherein, 1≤m≤200,1≤n≤500.
In addition, including the following steps: will be complete the invention also discloses a kind of synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin
Fluorine cyclobutyl arylene ether phenol polymer, hexafluoro bisphenol-a, phenyl-dihalide formonitrile HCN or dihalo para-Phthalonitrile, 4,4 '-difluorodiphenyls
Ketone and catalyst are 1:(1~6 in molar ratio): (1~3): (1~3): (2~3) are placed in the mixed solution of organic solvent and toluene
In, in N2Under stream effect, after carrying out temperature control reaction twice, reaction solution is poured into deionized water under stiring precipitate immediately, mistake
Filter, the sediment being obtained by filtration is impregnated with deionized water, primary every 4~8h replacement water, is filtered, will be soaked after repeating 5~8 times
Sediment after bubble is placed in freeze drying box dry 10h, obtains poly(aryl ether ketone) CABLE MATERIALS resin sample；The organic solvent is
N,N-dimethylacetamide, dimethyl sulfoxide or N-Methyl pyrrolidone.
Wherein, the temperature control twice reaction is prior to 110~160 DEG C 2~8h of reaction, react 2 then at 160~200 DEG C~
12h。
Wherein, the phenyl-dihalide formonitrile HCN is 2,5- dichlorobenzonitrile or 2,5- difluorobenzonitrile；The dihalo pair
Benzene dicarbonitrile is 2,5- dichloro para-Phthalonitrile or 2,5- dibromo para-Phthalonitrile.Wherein, the catalyst is Anhydrous potassium carbonate
Or natrium carbonicum calcinatum.Wherein, the synthesis of perfluorocyclobutanearyl aryl-ether phenol polymer includes the following steps: trifluoro vinyl aryl
Ether is dissolved in diphenyl ether, is placed in 160 DEG C of oil baths after polyase 13 h, and obtaining product is perfluorocyclobutanearyl aryl-ether polymer, is added
Enter trifluoro vinyl p-methoxyphenyl ether as end-capping reagent, the reaction was continued 7h terminates reaction, obtains end and contain methoxyl group
Perfluorocyclobutanearyl aryl-ether polymer, by with BBr3Reaction demethylation obtains end and contains perfluorocyclobutanearyl aryl-ether for hydroxyl
Phenol polymer.
Wherein, the molar feed ratio of the perfluorocyclobutanearyl aryl-ether and trifluoro vinyl p-methoxyphenyl ether is 2: 1.
The invention has the following beneficial effects:
1, the present invention synthesizes a kind of poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic method for the first time, develops a kind of novel cable
Material, the material effectively improve thermal stability, crystallinity and the dissolubility of polymer, and the dielectric for reducing polymer is normal
Number, dielectric dissipation factor, the rate of signal attenuation of High Speed Transfer frequency band, maintain the excellent properties of poly(aryl ether ketone) material, make
The poly(aryl ether ketone) material has the advantages that poly (arylene ether nitrile), polyether-ether-ketone and three kinds of materials containing fluorine structure simultaneously.
2, a kind of poly(aryl ether ketone) CABLE MATERIALS resin of the present invention and its synthetic method, the material have compared with corrosion-and high-temp-resistant
Energy, radiation hardness, flame retardant property have more crosslinking points.
3, a kind of poly(aryl ether ketone) CABLE MATERIALS resin of the present invention and its synthetic method, the signal of the material High Speed Transfer frequency band decline
Subtract smaller than the wire and cable of commercially available material, physical mechanical property also significantly improves.
4, a kind of synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin of the present invention, the synthetic method is simple, and synthetic yield is higher,
Production cost is low.
Detailed description of the invention
Fig. 1 is the IH-NMR spectrogram for the poly(aryl ether ketone) CABLE MATERIALS resin that the embodiment of the present invention 2 obtains；
Fig. 2 is the infrared spectrogram for the poly(aryl ether ketone) CABLE MATERIALS resin that the embodiment of the present invention 2 obtains.Specific embodiment
It is several embodiments of the present invention below, further illustrates the present invention, but the present invention is not limited only to this.
The synthesis of perfluorocyclobutanearyl aryl-ether phenol polymer: Trifluorovinyl Aryl Ethers are dissolved in diphenyl ether, are placed in
In 160 DEG C of oil baths after polyase 13 h, obtaining product is perfluorocyclobutanearyl aryl-ether polymer, and trifluoro vinyl is added to methoxybenzene
Base ether envelope is as end agent (molar ratio of monomer and end-capping reagent be 2:1), and the reaction was continued 7h is terminated and reacted, obtains end and contain
Have the perfluorocyclobutanearyl aryl-ether polymer of methoxyl group, by with BBr3Reaction demethylation obtains end and contains perfluor ring for hydroxyl
Butyl aryl ether phenol polymer, passes through gpc analysis: Mn=2450, PDI=1.25.Its synthetic route:
Embodiment 1
The synthesis of the synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 12.25g (5mmol) perfluor is sequentially added in conical flask
Cyclobutyl arylene ether phenol polymer, 5.04g (15mmol) hexafluoro bisphenol-a, 1.39g (10mmol) 2,5- difluorobenzonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
After filter, put the precipitate in freeze drying box 10 hours dry, obtain poly(aryl ether ketone) CABLE MATERIALS resin sample by GPC points
Analysis: Mn=46200, PDI=2.34, yield 96%.Its synthetic route:
Embodiment 2
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 24.50g (10mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 3.36g (10mmol) hexafluoro bisphenol-a, 1.39g (10mmol) 2,5- difluorobenzonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
47200, PDI=2.64, yield 98%, and poly(aryl ether ketone) sample manufactured in the present embodiment is shown by DSC result of study
Glass transition temperature is 185 DEG C, shows that the starting weightless temperature of synthesized sample is 496 DEG C by thermal gravimetric analysis results, weightless
5% temperature is 567 DEG C.In addition, also carrying out viscosity test to prepared sample, poly(aryl ether ketone) CABLE MATERIALS resin sample is existed
25 DEG C are dissolved in DMF, measure its viscosity, the results showed that 0.36dL/g.
Embodiment 3
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 24.50g (10mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 3.36g (10mmol) hexafluoro bisphenol-a, 0.82g (5mmol) 2,5- difluoro para-Phthalonitrile, 3.27g
(15mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
56580, PDI=2.75, yield 94.2%.Its synthetic route:
Embodiment 4
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 24.50g (10mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 3.36g (10mmol) hexafluoro bisphenol-a, 1.64g (10mmol) 2,5- difluoro para-Phthalonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
59810, PDI=2.93, yield 98%.
Embodiment 5
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 12.25g (5mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 5.04g (15mmol) hexafluoro bisphenol-a, 1.64g (10mmol) 2,5- difluoro para-Phthalonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
55810, PDI=2.53, yield 97%.
Embodiment 6
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 24.50g (10mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 3.36g (10mmol) hexafluoro bisphenol-a, 1.72g (10mmol) 2,5- dichlorobenzonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
47200, PDI=2.64, yield 97.8%.Its synthetic route:
Embodiment 7
The synthesis of poly(aryl ether ketone) CABLE MATERIALS resin: 24.50g (10mmol) perfluorocyclobutanearyl is sequentially added in conical flask
Aryl ether phenol polymer, 3.36g (10mmol) hexafluoro bisphenol-a, 1.97g (10mmol) 2,5- dichloro para-Phthalonitrile, 2.18g
(10mmol) 4,4 '-difluoro benzophenone, toluene 100mL, DMAc120mL, 5.53g (40mmol) potassium carbonate, in the N of 1mL/s2Stream
Lower 140 DEG C are reacted 3 hours, are then heated to 170 DEG C and are reacted 20 hours, immediately pour into reaction solution in deionized water under stiring
Precipitating, filtering.The sediment being obtained by filtration is impregnated with deionized water, it is primary every 3 hours replacement water, it is filtered after being repeated 7 times,
Drying 10 hours in freeze drying box are put the precipitate in, poly(aryl ether ketone) CABLE MATERIALS resin sample is obtained and passes through gpc analysis: Mn=
59810, PDI=2.93, yield 94.5%.Its synthetic route:
Fig. 1 is the IH-NMR spectrogram for the poly(aryl ether ketone) CABLE MATERIALS resin that the embodiment of the present invention 2 obtains.7.85ppm,
7.83ppm, 7.79ppm, 7.78ppm, 7.76ppm and 7.73ppm be cyano benzene monomer on hydrogen absorption peak, 7.42ppm,
7.14ppm, 7.23ppm and 7.22ppm are the absorption peak of hydrogen on phenyl ring in one monomers, 7.12ppm, 7.10ppm, 7.08ppm,
7.01ppm, 6.99ppm, 6.95ppm and 6.93ppm are the absorption peak of hydrogen on phenyl ring in phenol monomer.
Fig. 2 is the infrared spectrogram of the poly(aryl ether ketone) CABLE MATERIALS resin of embodiment 2.It can be seen from the figure that being in wave number
2936cm-1Place be phenyl ring on=C-H stretching vibration characteristic peak, in 3056cm-1、1649cm-1、1592cm-1、1496cm-1It is benzene
C=C double bond characteristic absorption peak, 1234cm on ring-1And 1161cm-1There is the characteristic absorption peak of Ar-O-Ar, 2217cm in place-1Out
The characteristic absorption peak of existing-CN, illustrates that difluoro cyano benzene, difluoro benzophenone and hexafluoro bisphenol-a react.
And Mn=47200, point of synthetic are become from perfluorocyclobutanearyl aryl-ether phenol Mn=2450 by gpc analysis
Son amount increases.
In conclusion provable perfluorocyclobutanearyl aryl-ether phenol polymer, hexafluoro bisphenol-a, 2,5- difluorobenzonitrile, 4,
Polycondensation reaction has occurred in 4 '-difluoro benzophenones, and itrile group and perfluorocyclobutanearyl aryl-ether are successfully introduced into poly(aryl ether ketone) main chain
In, synthesize the linear poly(aryl ether ketone) containing itrile group and perfluorocyclobutanearyl aryl-ether structure, a kind of novel poly(aryl ether ketone) cable
Expect resin.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (8)
1. a kind of poly(aryl ether ketone) CABLE MATERIALS resin, which is characterized in that structural formula is as follows:
M and n indicates the degree of polymerization, is positive integer.
2. a kind of poly(aryl ether ketone) CABLE MATERIALS resin as described in claim 1, it is characterised in that: 1≤m≤200,1≤n≤500.
3. a kind of synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 1 or 2, which is characterized in that including such as
Lower step: by perfluorocyclobutanearyl aryl-ether phenol polymer, hexafluoro bisphenol-a, phenyl-dihalide formonitrile HCN or dihalo para-Phthalonitrile, 4,
4 '-difluoro benzophenones and catalyst are 1:(1~6 in molar ratio): (1~3): (1~3): (2~3) are placed in organic solvent and first
In the mixed solution of benzene, in N2Under stream effect, after carrying out temperature control reaction twice, reaction solution is poured into deionization under stiring immediately
It is precipitated in water, filters, the sediment being obtained by filtration is impregnated with deionized water, it is primary every 4~8h replacement water, it repeats 5~8 times
After filter, the sediment after immersion is placed in freeze drying box dry 10h, obtains poly(aryl ether ketone) CABLE MATERIALS resin sample；Institute
Stating organic solvent is n,N-dimethylacetamide, dimethyl sulfoxide or N-Methyl pyrrolidone.
4. the synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 3, it is characterised in that: the temperature control twice is anti-
It should be prior to 110~160 DEG C 2~8h of reaction, then at 160~200 DEG C of 2~12h of reaction.
5. the synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 3, it is characterised in that: the phenyl-dihalide
Formonitrile HCN is 2,5- dichlorobenzonitrile or 2,5- difluorobenzonitrile；The dihalo para-Phthalonitrile is 2,5- dichloro para-Phthalonitrile
Or 2,5- dibromo para-Phthalonitrile.
6. the synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 3, it is characterised in that: the catalyst is nothing
Aqueous carbonate potassium or natrium carbonicum calcinatum.
7. the synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 3, it is characterised in that: perfluor cyclobutyl arylene
The synthesis of ether phenol polymer includes the following steps: for Trifluorovinyl Aryl Ethers to be dissolved in diphenyl ether, is placed in 160 DEG C of oil baths and gathers
After closing 3h, obtaining product is perfluorocyclobutanearyl aryl-ether polymer, and trifluoro vinyl p-methoxyphenyl ether is added as sealing end
Agent, the reaction was continued 7h terminate reaction, obtain the perfluorocyclobutanearyl aryl-ether polymer for containing methoxyl group in end, by with BBr3
Reaction demethylation obtains end and contains perfluorocyclobutanearyl aryl-ether phenol polymer for hydroxyl.
8. the synthetic method of poly(aryl ether ketone) CABLE MATERIALS resin as claimed in claim 7, it is characterised in that: the perfluorocyclobutanearyl
The molar feed ratio of aryl ether and trifluoro vinyl p-methoxyphenyl ether is 2: 1.
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| CN109824886A (en) * | 2018-12-29 | 2019-05-31 | 福州通尔达电线电缆有限公司 | One kind containing DOPO based structures unit poly(aryl ether ketone) CABLE MATERIALS resin and its synthetic method |
| CN109705335A (en) * | 2018-12-29 | 2019-05-03 | 福州通尔达电线电缆有限公司 | One kind containing itrile group and DOPO based structures ketone-grouped resin and its synthetic method |
| CN118085192A (en) * | 2024-04-23 | 2024-05-28 | 西南石油大学 | Shape memory poly (arylene ether nitrile) sieve tube material, preparation method and application thereof |
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Denomination of invention: A Polyaryletherketone Cable Material Resin and Its Synthesis Method Effective date of registration: 20230809 Granted publication date: 20190607 Pledgee: Agricultural Bank of China Limited Ninghua County Branch Pledgor: Fujian Chaoyang wire and cable Co.,Ltd. Registration number: Y2023350000179 |