Methods for degrading and recycling cross-linked polymers and reinforced polymer composites
A technology for strengthening composite materials and cross-linked polymers, which is applied in the direction of plastic recycling and recycling technology, and can solve the problems of strong corrosiveness, unsafety, and unfriendly environment of phenol, and achieve mild recovery conditions, stable quality, and easy control. Effect
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[0033] Example 1 Preparation of curing agent A
[0034]
[0035] 1000g of N-(2-hydroxyethyl)phthalimide, 157g of paraformaldehyde, 6.8g of anhydrous p-toluenesulfonic acid and 1.5 liters of toluene were mixed, and DEAN-STARK refluxed and separated water. After refluxing for 20 hours, the reaction is complete, and the temperature is reduced to room temperature. 2 liters of petroleum ether (boiling range: 60-90°C) is added to obtain a white precipitate, which is filtered, washed with 1 liter of petroleum ether, and the solid is dried to obtain 950 g of crude product. Add 3.4 Liter 20% NaOH solution, heat to reflux for 10 hours, cool, add chloroform / isopropanol (3:1) for extraction, separate the layers, dry the organic phase with anhydrous sodium sulfate, and distill under reduced pressure to obtain 200g of curing agent A (70Pa vacuum conditions The lower boiling range is 71-72°C).
Example Embodiment
[0036] Example 2 Preparation of curing agent B
[0037]
[0038] Put 80 g of toluene and 440 g of 3-chloroglycerin into the reaction flask, put in 548 g of chloroacetaldehyde dimethylacetal and 3 g of p-toluenesulfonic acid under stirring, the system slowly heated up, and Dean-Stark refluxed methanol for 12-16 hours. After the reaction is completed, the temperature is lowered to below 40°C, an appropriate amount of sodium carbonate is added to the reaction flask to adjust the pH value of the reaction liquid system to be nearly neutral, and then the reaction liquid is concentrated under reduced pressure, and all toluene is recovered to obtain 760 g of chlorinated intermediates.
[0039] Add 400 ml of N,N-dimethylformamide into a three-necked flask, put in 231g of phthalimide potassium salt and 86.5g of chlorinated intermediates under stirring, heat up to 150℃, and react for 8 hours. After the reaction is complete , Concentrate under reduced pressure to recover DMF. The residue is di...
Example Embodiment
[0040] Example 3 Preparation of curing agent C
[0041]
[0042] 89g 2-nitropropane, 30g paraformaldehyde and 100mL triethylamine were stirred and reacted at 45°C for 0.5 hour. The reaction mixture was filtered to obtain 60 g of 2-methyl-2-nitro-1-propanol.
[0043] Mix 11.9g 2-methyl-2-nitro-1-propanol, 5.7g 2,2-dimethoxypropane, 0.3g p-toluenesulfonic acid and 500mL cyclohexane, and extract and evaporate with Dean-Stark receiver Of methanol. After 6 hours, the solution was cooled to room temperature, an appropriate amount of sodium carbonate was added to the reaction flask, and then the reaction solution was concentrated under reduced pressure to obtain 5.7g 2-methyl-1-((2-(2-methyl-2-nitro Propoxy)isopropyl)oxy)-2-nitropropane.
[0044] Mix 1g of 2-methyl-1-((2-(2-methyl-2-nitropropoxy)isopropyl)oxy)-2-nitropropane, 0.1g Raney nickel and 25m methanol, Hydrogen was introduced for reduction reaction at 55°C for 12 hours, the reaction mixture was filtered, and the filtrate was co...
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