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A polyphenylene ether and dimethylphenol technology, applied in the field of polyphenylene ether preparation, can solve the problems of polyphenylene ether with large molecular weight, highly toxic solvents, and serious pollution
Inactive Publication Date: 2014-04-09
JINAN DEV ZONE XINGHUO SCI & TECH RES INST
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Abstract
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Problems solved by technology
The polyphenylene ether synthesized by this method has a large molecular weight, and most of the solvents are highly toxic and pollute seriously.
Method used
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Effect test
Embodiment 1
[0023] 1. Add 244g of 2,6-dimethylphenol, 7.3g of cuprous chloride, and 500ml of pyridine into the reactor, and then add 3.65L of mixed solvent (volume ratio 1,4-dioxane:water=7:1 ), stirring to dissolve;
[0024] 2. Slowly add 500ml of hydrogen peroxide to the reactor at room temperature, and the dropping time is controlled at 1h. After the titration is completed, continue to stir and react for 3h;
[0025] 3. After the reaction, pour the solution into a methanol solution containing 5% hydrochloric acid, and a pale yellow precipitate precipitates out. The precipitate was collected by suction filtration, washed three times with methanolic hydrochloric acid solution, and dried in vacuum to obtain white polyphenylene ether powder.
[0026] Yield 91.7%, weight average molecular weight M w =10271g / mol, number average molecular weight M n =2850 g / mol.
Embodiment 2
[0028] With embodiment 1, difference is:
[0029] In step (1), the volume ratio of the mixed solvent is 1,4-dioxane:water=2:1.
[0030] Yield 87.4%, weight average molecular weight M w =4255g / mol, number average molecular weight M n =1880 g / mol.
Embodiment 3
[0032] With embodiment 1, difference is:
[0033] In step (1), the volume ratio of the mixed solvent is 1,4-dioxane:water=1:2.
[0034] Yield 79.6%, weight average molecular weight M w =1766g / mol, number average molecular weight M n =935 g / mol.
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Abstract
The invention relates to the high molecular material field, and more specifically relates to a preparation method of polyphenyl ether. The preparation method of the polyphenyl ether comprises the following steps of adding cuprous chloride, pyridine and 2,6-xylenol to a reactor, and then adding the mixed solvent of 1,4-dioxane and water, and stirring for dissolving; slowly and dropwise adding hydrogen peroxide to the reactor at the room temperature, controlling the dropping time within 1-2h, and further stirring for reacting for 3-5h after finishing dropping; after the reaction is ended, pouring the solution into a methanol solution containing 5% of hydrochloric acid, carrying out suction filtration and collecting precipitate, washing for 3-5 times by using the hydrochloric acid-containing methanol solution, and drying in vacuum to obtain white polyphenyl ether powder. The mixed solvent employed by the preparation method provided by the invention is very effective for controlling the molecular weight of the polyphenyl ether; as the water content is increased and the dissolubility of the polyphenyl ether with high molecular weight is reduced, the polyphenyl ether precipitates as long as a certain molecular weight is achieved to terminate the reaction; the water content can be taken as the effective way to control the molecular weight; the ratio of the mixed solvent can be adjusted according to the desired molecular weight.
Description
technical field [0001] The invention relates to the field of macromolecular materials, in particular to a preparation method of polyphenylene ether. Background technique [0002] Polyphenylene ether (PPE) is a thermoplastic resin synthesized from 2,6-disubstituted phenol through oxidative coupling polymerization, generally in the form of khaki powder, and the most commonly used one is a polyphenylene ether synthesized from 2,6-dimethylphenol. Phenyl ether has excellent comprehensive properties. Its molecular structure determines that this kind of engineering material has good thermodynamic properties. It can work continuously in the temperature range of -160~190°C, and its thermal creep at high temperature is the best among all thermoplastic engineering materials. PPE can maintain good electrical properties and mechanical properties in a wide temperature range, and can maintain good tensile strength and creep resistance even at high temperatures, low water absorption and e...
Claims
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