Hydrogenation method for increasing yield of cyclohexane-1,4-dicarboxylic acid diisooctyl ester
US-2020172463-A1 · Jun 4, 2020 · US
US12110365B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-12110365-B2 |
| Application number | US-202217739212-A |
| Country | US |
| Kind code | B2 |
| Filing date | May 9, 2022 |
| Priority date | Mar 2, 2022 |
| Publication date | Oct 8, 2024 |
| Grant date | Oct 8, 2024 |
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A method for producing polyphenylene ether amine includes following steps. In step (a), a hydrogenation reaction tank is provided; a guided gas stirrer is disposed in the hydrogenation reaction tank. In step (b), a reaction solution is placed in the hydrogenation reaction tank, and the reaction solution is nitro polyphenylene ether dissolved in a solvent. In step (c), a hydrogenation catalyst is added to the reaction solution. In step (d), a hydrogen gas is introduced into the hydrogenation reaction tank. In step (e), the guided gas stirrer is activated. In step (f), a hydrogenation reaction is carried out on the conditions that a reaction temperature is 50-200 degrees Celsius and a reaction time is 1-20 hours, so as to hydrogenate the nitro polyphenylene ether in the reaction solution to polyphenylene ether amine. In step (g), the reaction solution is cooled down to a room temperature; the hydrogenation catalyst is removed.
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What is claimed is: 1. A method for producing polyphenylene ether amine, the method comprising following steps: step (a): providing a hydrogenation reaction tank with a guided gas stirrer adapted to perform gas extracting, gas exhausting, and stirring functions, wherein the guided gas stirrer comprises a hollow rotation shaft and a vane disposed at an end of the hollow rotation shaft, and the hollow rotation shaft has a gas extracting hole and a gas exhausting hole; step (b): placing a reaction solution in the hydrogenation reaction tank, wherein the reaction solution is nitro polyphenylene ether dissolved in a solvent; step (c): adding a hydrogenation catalyst to the reaction solution, wherein a usage amount of the hydrogenation catalyst is 0.2-15 weight percentage of the nitro polyphenylene ether; step (d): introducing a hydrogen gas into the hydrogenation reaction tank, so that a hydrogen pressure in the hydrogenation reaction tank is 10-120 bars; step (e): activating the guided gas stirrer, so that the hollow rotation shaft in the guided gas stirrer reaches a predetermined rotation speed to drive the vane to stir the reaction solution, wherein the hollow rotation shaft introduces the hydrogen gas from a top of the reaction solution through the gas extracting hole of the hollow rotation shaft and transmits the hydrogen gas into the reaction solution through the gas exhausting hole of the hollow rotation shaft, and the hydrogen gas in the reaction solution is stirred by the vane and evenly distributed; step (f): carrying out a hydrogenation reaction, wherein a reaction temperature is 50-200 degrees Celsius, and a reaction time is 1-20 hours to hydrogenate the nitro polyphenylene ether in the reaction solution to the polyphenylene ether amine; and step (g): cooling down the reaction solution to a room temperature and removing the hydrogenation catalyst, wherein the hydrogenation catalyst comprises a palladium catalyst. 2. The method for producing the polyphenylene ether amine according to claim 1 , wherein in the step (c), the usage amount of the hydrogenation catalyst is 0.5-10 weight percentage of the nitro polyphenylene ether. 3. The method for producing the polyphenylene ether amine according to claim 1 , wherein in the step (d), the hydrogenation reaction tank has an internal hydrogen pressure of 10-120 bars after the hydrogen gas is introduced. 4. The method for producing the polyphenylene ether amine according to claim 1 , wherein in the step (e), the predetermined rotation speed reached by the hollow rotation shaft and the vane is 1200-1500 rpm. 5. The method for producing the polyphenylene ether amine according to claim 1 , wherein in the step (f), the reaction temperature at which the hydrogenation reaction is carried out is 70-180 degrees Celsius. 6. The method for producing the polyphenylene ether amine according to claim 1 , wherein a heat exchange plate or a coil is further disposed in the hydrogenation reaction tank.
moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title
Plates; Cylinders · CPC title
Heating or cooling the reactor · CPC title
Coils · CPC title
by oxidation of phenols · CPC title
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