CN114292397A - Polyphenylene ether resin purification process - Google Patents
Polyphenylene ether resin purification process Download PDFInfo
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- CN114292397A CN114292397A CN202111627638.4A CN202111627638A CN114292397A CN 114292397 A CN114292397 A CN 114292397A CN 202111627638 A CN202111627638 A CN 202111627638A CN 114292397 A CN114292397 A CN 114292397A
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- ether resin
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- polyphenylene ether
- dimethylphenol
- dodecyl sulfate
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- 239000011347 resin Substances 0.000 title claims abstract description 37
- 229920005989 resin Polymers 0.000 title claims abstract description 37
- 238000000746 purification Methods 0.000 title claims abstract description 15
- 229920001955 polyphenylene ether Polymers 0.000 title claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- NXXYKOUNUYWIHA-UHFFFAOYSA-N 2,6-Dimethylphenol Chemical compound CC1=CC=CC(C)=C1O NXXYKOUNUYWIHA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000004821 distillation Methods 0.000 claims abstract description 21
- ODJUOZPKKHIEOZ-UHFFFAOYSA-N 4-[2-(4-hydroxy-3,5-dimethylphenyl)propan-2-yl]-2,6-dimethylphenol Chemical compound CC1=C(O)C(C)=CC(C(C)(C)C=2C=C(C)C(O)=C(C)C=2)=C1 ODJUOZPKKHIEOZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 12
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229920013636 polyphenyl ether polymer Polymers 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 28
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229940079895 copper edta Drugs 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 17
- 229920006380 polyphenylene oxide Polymers 0.000 abstract description 17
- 229960001484 edetic acid Drugs 0.000 abstract 3
- 238000007334 copolymerization reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Polyethers (AREA)
Abstract
The invention discloses a polyphenylene oxide resin purification process, which comprises the following raw materials of tetramethyl bisphenol A, 2,6 dimethylphenol, sodium dodecyl sulfate, sodium hydroxide, copper chloride and EDTA (ethylene diamine tetraacetic acid), wherein the ratio of the tetramethyl bisphenol A to the 2,6 dimethylphenol to the sodium dodecyl sulfate to the sodium hydroxide is 2: 20: 5: 2, the ratio of the copper chloride to the EDTA is 1: 1. the polyphenyl ether resin purification process adopts a reaction kettle low-pressure distillation process, can reduce the residual quantity of unreacted 2, 6-dimethylphenol and tetramethyl bisphenol A, simultaneously can better uniformly heat and control the temperature compared with a screw extruder, prevents reaction dead angles, greatly improves batch stability and quality stability, and solves the problem of unstable product quality in the prior art.
Description
Technical Field
The invention relates to the technical field of high molecular compound synthesis, in particular to a polyphenylene ether resin purification process.
Background
In the coming 5G communication era, terminal electronic and electrical equipment and derivative application scenes also need to be upgraded and replaced, and the copper-clad plate in the 5G era tends to be designed with more layers of high integration, so that new requirements are provided for the copper-clad plate base material, better transmission performance and heat dissipation performance are needed, and the copper-clad plate is meant to use electronic base materials with higher frequency, higher transmission speed and better heat resistance. At present, under the trend of high-speed and high-frequency PCB, the mainstream copper-clad plate materials comprise polytetrafluoroethylene resin (PTFE), epoxy resin (EP), bismaleimide triazine resin (BT), cyanate resin (CE), polyphenylene oxide resin (PPO) and polyimide resin (PI), which have a common characteristic, and the dielectric constant and the dielectric loss of the resin are low or low.
Polyphenylene Oxide (PPO) is one of five general engineering plastics in the world, and is thermoplastic engineering plastic with excellent comprehensive performance. Because PPO has excellent electrical property, mechanical property, moisture resistance and dimensional stability, PPO is one of the materials with the most excellent comprehensive properties in the copper-clad plate substrate materials. The high-performance glass fiber reinforced plastic composite material has the advantages of excellent mechanical property, low dielectric constant (epsilon is 2.45 under 1 MHz), low dielectric loss tangent (0.0008-0.0042, almost free of temperature, humidity and frequency influence), high glass transition temperature (Tg is as high as 210 ℃), good flame retardant property (oxygen index is 29, self-extinguishing property is achieved), good size stability and the like, low water absorption (saturated water absorption at room temperature is less than 0.05%), low relative density, acid and alkali resistance, and the like. However, polyphenylene oxide has a relatively high molecular weight, a high melt viscosity, and poor solubility in solvents, resulting in poor processability; and the solvent resistance of thermoplastic polyphenyl ether is poor, stress cracking can occur in mineral oil, ketone or ester solvents, and halogenated aliphatic hydrocarbon and aromatic hydrocarbon solvents such as dichloroethane, toluene and the like can cause the polyphenyl ether to swell or dissolve, so that the polyphenyl ether is greatly limited in industrial application. In order to overcome the disadvantages of high melting temperature and melt viscosity of PPO resin due to high molecular weight, the development and research of low molecular weight PPO are gradually paid attention to. The low molecular weight PPO not only retains the excellent dielectric property, mechanical property, heat resistance and chemical stability of the PPO resin, but also has the advantages of low viscosity, high fluidity, good compatibility with other resins and the like. Particularly, the low molecular weight PPO (PPO-2OH) with double-end hydroxyl groups can be further modified and modified to prepare telechelic type, block type, graft type and star type polymers due to the active hydroxyl groups at the two ends. The preparation of the low molecular weight PPO-2OH mainly comprises a coupling method, a monomer copolymerization method and a redistribution reaction method. The coupling method is to prepare the low molecular weight PPO and the biphenyl biquinone compound through coupling reaction. The monomer copolymerization is obtained by taking pure 2, 6-dimethylphenol or a mixture of the pure 2, 6-dimethylphenol, bisphenol A and aromatic diol as raw materials and carrying out oxidative copolymerization under the action of oxygen and a catalyst. Redistribution rule refers to the process by which high molecular weight PPO is depolymerized to low molecular weight PPO under the action of a redistribution agent and a catalyst. The three methods have advantages and disadvantages, and are mainly applicable to the production of the copper-clad plate by adopting a monomer copolymerization method at present. The direct monomer copolymerization method has simple process, but the purity of the monomer is not high due to side reaction, and a screw extruder is usually adopted for purification and granulation, so that the product has more impurities and poor performance.
At present, the synthesis control of the double-end hydroxyl low molecular weight polyphenylene ether is difficult, and the product has the defects of poor batch stability and unstable quality. These all add to the difficulty of large-scale industrial application of low molecular weight PPO-2OH, which requires further intensive research and improvement. Therefore, a polyphenylene ether resin purification process is needed to improve batch stability and quality stability and solve the problem of unstable product quality in the prior art.
Disclosure of Invention
The invention aims to provide a polyphenylene ether resin purification process to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the polyphenylene oxide resin purification process comprises the following raw materials in parts by weight of tetramethyl bisphenol A, 2,6 dimethylphenol, sodium dodecyl sulfate, sodium hydroxide, copper chloride and EDTA, wherein the ratio of the tetramethyl bisphenol A to the 2,6 dimethylphenol to the sodium dodecyl sulfate to the sodium hydroxide is 2: 20: 5: 2, the ratio of the copper chloride to the EDTA is 1: 1.
further, the method comprises the following steps:
(1) 1g of 2, 6-dimethyl bisphenol, 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen at the flow rate of 2ml/min, and reacting at normal temperature;
(3) after the reaction is finished, adding citric acid for neutralization reaction, adding sodium chloride for precipitation and demulsification, and filtering to obtain white powder;
(4) and adding the obtained powder into a distillation kettle, vacuumizing and heating, heating for 1 hour for the first time to remove water, and heating for the second time to remove 2, 6-dimethylphenol in the polyphenyl ether resin to obtain the polyphenyl ether resin with the purity of 99.9 percent.
Further, the normal temperature reaction in the step (2) needs to be continuously performed for 24 hours.
Further, the first heating in the step (4) needs to be continuously performed at 100 ℃.
Further, the second heating in the step (4) needs to be continuously performed at a temperature of 230 ℃ and 250 ℃.
Further, the second heating in the step (4) needs to be performed for 1 to 10 hours.
Compared with the prior art, the invention has the beneficial effects that: the polyphenyl ether resin purification process adopts a reaction kettle low-pressure distillation process, can reduce the residual quantity of unreacted 2, 6-dimethylphenol and tetramethyl bisphenol A, simultaneously can better uniformly heat and control the temperature compared with a screw extruder, prevents reaction dead angles, greatly improves batch stability and quality stability, and solves the problem of unstable product quality in the prior art.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one, purification was performed by the following steps:
(1) 1g of 2, 6-dimethyl bisphenol A and 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen with the flow rate of 2ml/min, and reacting for 24 hours at normal temperature;
(3) after the reaction is finished, adding citric acid for neutralization reaction, adding sodium chloride for precipitation and demulsification, and filtering to obtain white powder;
(4) adding the obtained powder into a distillation kettle, vacuumizing and heating the distillation kettle, heating the distillation kettle at 100 ℃ for 1 hour to remove water, continuously heating the distillation kettle to 230 ℃ and 250 ℃ for 5 hours to remove 2, 6-dimethylphenol in the polyphenylene ether resin to obtain the polyphenylene ether resin with the purity of 99.9 percent.
Example two, purification was performed by the following steps:
(1) 1g of 2, 6-dimethyl bisphenol A and 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen with the flow rate of 2ml/min, and reacting for 24 hours at normal temperature;
(3) after the reaction is finished, adding citric acid for neutralization reaction, adding sodium chloride for precipitation and demulsification, and filtering to obtain white powder;
(4) adding the obtained powder into a distillation kettle, vacuumizing and heating the distillation kettle, heating the distillation kettle at 100 ℃ for 1 hour to remove water, continuously heating the distillation kettle to 230 ℃ and 250 ℃ for 1 hour to remove 2, 6-dimethylphenol in the polyphenylene ether resin to obtain the polyphenylene ether resin with the purity of 99 percent.
Example three, purification was performed by the following steps:
(1) 1g of 2, 6-dimethyl bisphenol A and 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen with the flow rate of 2ml/min, and reacting for 24 hours at normal temperature;
(3) after the reaction is finished, adding citric acid for neutralization reaction, adding sodium chloride for precipitation and demulsification, and filtering to obtain white powder;
(4) adding the obtained powder into a distillation kettle, vacuumizing and heating the distillation kettle, heating the distillation kettle at 100 ℃ for 1 hour to remove water, continuously heating the distillation kettle to 230 ℃ and 250 ℃ for 10 hours to remove 2, 6-dimethylphenol in the polyphenylene ether resin to obtain the polyphenylene ether resin with the purity of 99.9 percent.
As can be seen from the above examples, the length of heating time leads to different results.
Comparative example one, purification was performed by the following steps:
(1) 1g of 2, 6-dimethyl bisphenol A and 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen with the flow rate of 2ml/min, reacting for 24 hours at normal temperature, adding citric acid for neutralization reaction after the reaction is finished, adding sodium chloride for demulsification, and filtering to obtain white powder;
(4) the obtained powder was put into a still, and heated under vacuum at 100 ℃ for 1 hour to remove water, thereby obtaining a polyphenylene ether resin having a purity of 9.
The performance of the first, second and third examples is compared with that of the first comparative example, and the test items, test methods and results are shown in the following table:
| test items | Comparative example 1 | Example one | Example two | EXAMPLE III |
| Purity of | 98％ | 99.9％ | 99％ | 99.9％ |
In conclusion, it is understood that the polyphenylene ether resin with a purity of 99.9% can be obtained by adding the polyphenylene ether resin into a distillation kettle, vacuumizing and heating the distillation kettle, wherein twice heating is required, heating the distillation kettle at 100 ℃ for 1 hour to remove water, further heating the distillation kettle to 230 ℃ and 250 ℃ and heating the distillation kettle for 5 or 10 hours to remove 2, 6-dimethylphenol in the polyphenylene ether resin. Such as conventional heating only once, is not desirable.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A polyphenylene ether resin purification process, wherein the raw materials used comprise: the adhesive comprises tetramethyl bisphenol A, 2,6 dimethylphenol, sodium dodecyl sulfate, sodium hydroxide, copper chloride and EDTA, wherein the ratio of the tetramethyl bisphenol A to the 2,6 dimethylphenol to the sodium dodecyl sulfate to the sodium hydroxide is 2: 20: 5: 2, the ratio of the copper chloride to the EDTA is 1: 1.
2. the process for purifying a polyphenylene ether resin according to claim 1, comprising the following steps:
(1) 1g of 2, 6-dimethyl bisphenol, 0.1g of tetramethyl bisphenol A, 0.25g of sodium dodecyl sulfate and 0.1g of sodium hydroxide are added into a 500ml three-neck flask and dissolved in 200ml of water;
(2) then adding 0.01g/ml of copper chloride and EDTA complex aqueous solution, introducing oxygen at the flow rate of 2ml/min, and reacting at normal temperature;
(3) after the reaction is finished, adding citric acid for neutralization reaction, adding sodium chloride for precipitation and demulsification, and filtering to obtain white powder;
(4) and adding the obtained powder into a distillation kettle, vacuumizing and heating, heating for 1 hour for the first time to remove water, and heating for the second time to remove 2, 6-dimethylphenol in the polyphenyl ether resin to obtain the polyphenyl ether resin with the purity of 99.9 percent.
3. The process for purifying a polyphenylene ether resin according to claim 2, wherein: the normal temperature reaction in the step (2) needs to be continued for 24 hours.
4. The process for purifying a polyphenylene ether resin according to claim 2, wherein: the first heating in the step (4) needs to be continuously performed at 100 ℃.
5. The process for purifying a polyphenylene ether resin according to claim 2, wherein: the second heating in the step (4) needs to be continuously carried out at the temperature of 230 ℃ and 250 ℃.
6. The process for purifying a polyphenylene ether resin according to claim 2, wherein: the second heating in the step (4) needs to be continuously performed for 1 to 10 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080071059A1 (en) * | 2004-09-13 | 2008-03-20 | Waseda University | Process for Preparing Polyphenylene Ether |
| CN101497693A (en) * | 2009-02-19 | 2009-08-05 | 浙江大学 | Metallic ion-polyamide polyamide-amine complex compound catalyst and use for preparing polyphenylene oxide in aqueous medium |
| CN101497692A (en) * | 2009-02-19 | 2009-08-05 | 浙江大学 | Magnetic supported catalyst and use thereof in polyphenylene oxide preparation |
| CN101942087A (en) * | 2010-07-12 | 2011-01-12 | 浙江大学 | Metal ion-hyperbranched polyamide amine complex catalyst and application to preparing polyphenylene oxide (PPO) in water medium |
| CN113493565A (en) * | 2020-04-02 | 2021-10-12 | 上海孛柯博科技有限公司 | Polyphenyl ether, preparation method thereof and device for producing polyphenyl ether |
-
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- 2021-12-28 CN CN202111627638.4A patent/CN114292397A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080071059A1 (en) * | 2004-09-13 | 2008-03-20 | Waseda University | Process for Preparing Polyphenylene Ether |
| CN101497693A (en) * | 2009-02-19 | 2009-08-05 | 浙江大学 | Metallic ion-polyamide polyamide-amine complex compound catalyst and use for preparing polyphenylene oxide in aqueous medium |
| CN101497692A (en) * | 2009-02-19 | 2009-08-05 | 浙江大学 | Magnetic supported catalyst and use thereof in polyphenylene oxide preparation |
| CN101942087A (en) * | 2010-07-12 | 2011-01-12 | 浙江大学 | Metal ion-hyperbranched polyamide amine complex catalyst and application to preparing polyphenylene oxide (PPO) in water medium |
| CN113493565A (en) * | 2020-04-02 | 2021-10-12 | 上海孛柯博科技有限公司 | Polyphenyl ether, preparation method thereof and device for producing polyphenyl ether |
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Inventor after: Zhu Yongxiang Inventor after: Chen Xudong Inventor after: Xu Hongwu Inventor after: Li Xiaopeng Inventor before: Chen Xudong Inventor before: Zhu Yongxiang Inventor before: Xu Hongwu Inventor before: Li Xiaopeng |
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Application publication date: 20220408 |