CN104151542A - Bromine-containing polyphenylether resin and preparation method thereof - Google Patents
Bromine-containing polyphenylether resin and preparation method thereof Download PDFInfo
- Publication number
- CN104151542A CN104151542A CN201310178671.2A CN201310178671A CN104151542A CN 104151542 A CN104151542 A CN 104151542A CN 201310178671 A CN201310178671 A CN 201310178671A CN 104151542 A CN104151542 A CN 104151542A
- Authority
- CN
- China
- Prior art keywords
- polyphenylene oxide
- oxide resin
- preparation
- bromine
- brominated polyphenylene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a bromine-containing polyphenylether resin and a preparation method thereof, and belongs to the technical field of high-molecular materials. The preparation method comprises the following steps: adding 2000-3000 grams of methylbenzene to a three-neck flask with a stirrer, and then adding 25-50 grams of N-N dimethyl n-butylamine and 0.1-0.2 mol of cuprous chloride; stirring, then slowly adding 3-5 mol of 2-methyl-6 bromophenol at 50-60 DEG C, blowing air into the three-neck flask at the same time, keeping reflux reaction for 2-3 hours, then cooling, and filtering; then washing by using methanol for multiple times, and then placing into a drying oven for drying to obtain a crude bromine-containing polyphenylether resin product; dissolving the crude bromine-containing polyphenylether resin product into trichloromethane, stirring and refluxing for 1.5-2 hours in a heating state, then cooling, and then pouring into the methanol with volume doubled for precipitation; and filtering and washing to obtain a finished product. The bromine-containing polyphenylether resin disclosed by the invention can outstandingly improve the flame retardance and has good heat resistance and dimensional stability. The preparation method disclosed by the invention is short in process step and non-severe in operational process.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of brominated polyphenylene oxide resin, and relate to its preparation method.
Background technology
Polyphenylene oxide resin has excellent thermotolerance and dimensional stability and has certain flame retardant resistance.But, while using merely polyphenylene oxide resin article of manufacture, be difficult to obtain desirable flame retardant resistance effect, be mainly because the flame retardant resistance of polyphenylene oxide resin is not high.The mechanism that polyphenylene oxide resin stops burning is due to the easy carbon distribution of polyphenylene oxide, and contacting of isolated and oxygen, can not proceed combustion reactions, has positive effect so utilize this mechanism of polyphenylene oxide resin to develop the more excellent polyphenylene oxide resin of flame retardant effect.
Summary of the invention
Task of the present invention is to provide a kind of and contributes to significantly to improve flame retardant effect and use the safety in utilization that improves goods and the brominated polyphenylene oxide resin that is conducive to ensure good thermotolerance and dimensional stability.
Another task of the present invention is to provide a kind of preparation method of brominated polyphenylene oxide resin, and the method technique is terse, preparation requires not harsh and can ensure that the brominated polyphenylene oxide resin obtaining has flame retardant resistance, thermotolerance and the dimensional stability of standing out from one's fellows.
Task of the present invention completes like this, a kind of brominated polyphenylene oxide resin, and its structural formula is:
Another task of the present invention completes like this, and a kind of preparation method of brominated polyphenylene oxide resin, comprises the following steps:
A) prepare crude product, in the there-necked flask with agitator, add 2000-3000 gram of toluene, then add the cuprous chloride of 25-50 gram of N-N dimethyl-n-butylamine and 0.1-0.2mol, after stirring, under 50-60, DEG C slowly add 3-5mol2-methyl-6 bromophenol, in there-necked flask, blast air simultaneously, cooling after maintenance back flow reaction 2-3h, and filter, after then repeatedly washing with methyl alcohol, put into oven drying, obtain brominated polyphenylene oxide resin crude product;
B) prepare finished product, brominated polyphenylene oxide resin crude product is dissolved in trichloromethane, stirring and refluxing 1.5-2 hour under heated condition, then carries out coolingly, then pours in the methyl alcohol of two volumes and precipitates, and after filtration washing, obtains brominated polyphenylene oxide resin.
Technical scheme provided by the invention, owing to containing bromo element on molecular backbone chain, therefore can significantly be improved flame retardant resistance, and have good thermotolerance and dimensional stability; The preparation method who provides not only processing step is brief, and operating process is not harsh.
Embodiment
Embodiment 1:
A) prepare crude product, in the there-necked flask with agitator, add 2000 grams of toluene, then add the cuprous chloride of 25 grams of N-N dimethyl-n-butylamine and 0.1mol, after stirring, at 50 DEG C, add slowly 3mol2-methyl-6 bromophenol, in 60 minutes, add, in there-necked flask, blast air, keep back flow reaction cooling after 2 hours, and filter simultaneously, then after repeatedly washing with methyl alcohol, put into oven drying, obtain brominated polyphenylene oxide resin crude product.
B) prepare finished product, by by steps A) the brominated polyphenylene oxide resin crude product that obtains is dissolved in trichloromethane, stirring and refluxing reaction 2 hours under heated condition, then carry out cooling, then pour in the methyl alcohol of two volumes and precipitate, after filtration washing, obtain brominated polyphenylene oxide resin.On the molecular backbone chain of this brominated polyphenylene oxide resin, contain bromo element, structural formula is as follows:
Embodiment 2:
A) prepare crude product, in the there-necked flask with agitator, add 3000 grams of toluene, then add the cuprous chloride of 50 grams of N-N dimethyl-n-butylamine and 0.2mol, after stirring, add slowly 5mol2-methyl-6 bromophenol at 60 DEG C, in 50 minutes, add, in there-necked flask, blast air simultaneously, keep back flow reaction cooling after 3 hours, and filter, after then repeatedly washing with methyl alcohol, put into oven drying, obtain brominated polyphenylene oxide resin crude product.
B) prepare finished product, by by steps A) the brominated polyphenylene oxide resin crude product that obtains is dissolved in trichloromethane, stirring and refluxing reaction 1.5 hours under heated condition, then carry out cooling, then pour in the long-pending methyl alcohol of triploid and precipitate, after filtration washing, obtain brominated polyphenylene oxide resin.All the other are all with the description to embodiment 1.
Claims (2)
1. a brominated polyphenylene oxide resin, is characterized in that its structural formula is:
。
2. a preparation method for brominated polyphenylene oxide resin as claimed in claim 1, is characterized in that comprising the following steps:
A) prepare crude product, in the there-necked flask with agitator, add 2000-3000 gram of toluene, then add the cuprous chloride of 25-50 gram of N-N dimethyl-n-butylamine and 0.1-0.2mol, after stirring, under 50-60, DEG C slowly add 3-5mol 2-methyl-6 bromophenol, in there-necked flask, blast air simultaneously, cooling after maintenance back flow reaction 2-3h, and filter, after then repeatedly washing with methyl alcohol, put into oven drying, obtain brominated polyphenylene oxide resin crude product;
B) prepare finished product, brominated polyphenylene oxide resin crude product is dissolved in trichloromethane, stirring and refluxing 1.5-2 hour under heated condition, then carries out coolingly, then pours in the methyl alcohol of two volumes and precipitates, and after filtration washing, obtains brominated polyphenylene oxide resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310178671.2A CN104151542A (en) | 2013-05-14 | 2013-05-14 | Bromine-containing polyphenylether resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310178671.2A CN104151542A (en) | 2013-05-14 | 2013-05-14 | Bromine-containing polyphenylether resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104151542A true CN104151542A (en) | 2014-11-19 |
Family
ID=51877183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310178671.2A Pending CN104151542A (en) | 2013-05-14 | 2013-05-14 | Bromine-containing polyphenylether resin and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104151542A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243345A (en) * | 2016-08-04 | 2016-12-21 | 潍坊鑫洋化工有限公司 | A kind of novel brominated polyphenylether synthesis technique |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3793246A (en) * | 1970-12-18 | 1974-02-19 | Asahi Dow Ltd | Process for producing aromatic polyethers |
| US3825521A (en) * | 1971-07-31 | 1974-07-23 | Asahi Dow Ltd | Manganese amine chelate catalyzed aromatic polyether formation |
| US4483958A (en) * | 1977-09-27 | 1984-11-20 | Asahi-Dow Limited | Thermoplastic polymer compositions comprising aromatic polyether and an inorganic filler |
| JP2005333698A (en) * | 2004-05-18 | 2005-12-02 | Kaneka Corp | Polyphenylene ether based buried pipe |
| CN102002159A (en) * | 2010-11-05 | 2011-04-06 | 中国蓝星（集团）股份有限公司 | Method for preparing polyphenyl ether |
-
2013
- 2013-05-14 CN CN201310178671.2A patent/CN104151542A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3793246A (en) * | 1970-12-18 | 1974-02-19 | Asahi Dow Ltd | Process for producing aromatic polyethers |
| US3825521A (en) * | 1971-07-31 | 1974-07-23 | Asahi Dow Ltd | Manganese amine chelate catalyzed aromatic polyether formation |
| US4483958A (en) * | 1977-09-27 | 1984-11-20 | Asahi-Dow Limited | Thermoplastic polymer compositions comprising aromatic polyether and an inorganic filler |
| JP2005333698A (en) * | 2004-05-18 | 2005-12-02 | Kaneka Corp | Polyphenylene ether based buried pipe |
| CN102002159A (en) * | 2010-11-05 | 2011-04-06 | 中国蓝星（集团）股份有限公司 | Method for preparing polyphenyl ether |
Non-Patent Citations (1)
| Title |
|---|
| 师洪俊等: "《合成树脂及塑料技术全书》", 30 April 2006, 中国石化出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243345A (en) * | 2016-08-04 | 2016-12-21 | 潍坊鑫洋化工有限公司 | A kind of novel brominated polyphenylether synthesis technique |
| CN106243345B (en) * | 2016-08-04 | 2018-11-30 | 潍坊鑫洋化工有限公司 | A kind of brominated polyphenylether synthesis technology |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104262929B (en) | Fire retardation PC/ABS composite material of a kind of frequency electromagnetic waves shielding and preparation method thereof | |
| CN102399323B (en) | N,O-single ligand metal catalyst with stereochemical structure and preparation method thereof | |
| CN105086449B (en) | Phosphorus-containing POSS (polyhedral oligomeric silsesquioxane) flame-retardant bismaleimide resin and preparation method thereof | |
| CN104017210A (en) | Long-chain type metal coordination intumescent flame retardant and preparation method thereof | |
| CN103497336A (en) | Soluble polyimide with tertiary butyl and non-coplanar structure and preparation method thereof | |
| CN105693539A (en) | High-planarity diamine monomer containing fluorene or fluorenone structure and synthesis method and application thereof | |
| CN104151542A (en) | Bromine-containing polyphenylether resin and preparation method thereof | |
| CN104084063A (en) | Sulfonated poly(ether ether ketone)-amino loaded chromium organic skeleton hybrid membrane, and preparation and application thereof | |
| US20220315518A1 (en) | Preparation method of rhodium octanoate dimer | |
| CN110669295A (en) | Preparation method of high-heat-resistance polybutylene-1 composite tube material for conveying high-temperature fluid | |
| CN102167683B (en) | Bivalent cation magnetic ionic liquids and preparation method thereof | |
| CN103709348A (en) | Production method for anti-ablation temperature-resistant phenolic resin | |
| CN105481888A (en) | Metal organic frame material used for visible light photocatalysis, and synthetic method and application thereof | |
| CN104529715A (en) | Preparation method of 3,3',5,5'-tetraalkyl-4,4'-biphenol | |
| CN104945622B (en) | Ferrocene based flame retardant char-forming polymer and preparation method thereof | |
| CN101891603B (en) | 2,6-difluorobenzil and preparation method as well as application threreof | |
| WO2021043142A1 (en) | Mesoporous silicon resin flame retardant, preparation method therefor and flame retardant composite material thereof | |
| CN102617637A (en) | Preparation method of organophosphorus nitrogen system flame retardant with hydroquinone phosphate ester serving as framework | |
| CN103214674B (en) | Method for efficiently producing an organic silicone resin microsphere | |
| CN105272885A (en) | Method for preparation of novel adamantane derivative | |
| CN106588796A (en) | Aromatic primary diamine containing triaryl-s-triazine structure and ether bond and preparation method thereof | |
| CN105541896A (en) | Caprolactamyl silane and preparation method thereof | |
| CN102167906B (en) | Flame-retardant bismaleimide resin and preparation method thereof | |
| CN102887968B (en) | Non-metallocene bimetallic catalytic system for synthesizing broad/bimodal polyethylene and application thereof | |
| CN203663804U (en) | Novel device for high boiling pyrolysis of organic silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141119 |