Tripiperazine-triazine based charcoal forming agent and preparation method thereof
A charcoal-forming agent and piperazine technology, applied in the field of macromolecular charcoal-forming agent and its preparation, can solve problems such as difficult removal and uncontrollable product structure, and achieve fast reaction speed, mild and controllable preparation process, and high charcoal-forming rate Effect
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Embodiment 1
[0043] Example 1: Preparation of carbon-forming agent based on tripiperazine-triazine structure according to the following steps
[0044] (1) Preparation of Boc-piperazine: take 4.31g (0.05mol) of piperazine and add 100ml of CH at 25°C 2 Cl 2 In the solution, stir in a 250ml three-necked flask at a speed of 300r / min until uniform; 5.45g (0.025mol) of di-tert-butyl dicarbonate (Boc reagent) is dissolved in 50ml of CH 2 Cl 2 The solution is placed in a constant pressure dropping funnel; after the piperazine is dissolved, the Boc solution is added dropwise to the piperazine solution at a rate of 1-2 drops / s, and the temperature of the system is controlled at 25 ° C, and continues after the addition is complete. The reaction was carried out for 20h, and the reaction end was monitored by TLC; a white precipitate would be produced during the dropwise addition. After the reaction was completed, the product was suction filtered to remove the white precipitate and washed with water;...
Embodiment 2
[0049] Embodiment 2: step (1)-step (3) is the same as embodiment 1; wherein, the preparation of step (4) prepolymer A2: take 2.40g (0.04mol) of ethylenediamine and add 60ml NMP solution at 20°C , while adding acid binding agent pyridine 0.95g (0.012mol) and 5g CaCl 2 Stir in the three-necked flask at a speed of 300 r / min until uniform, and the system is connected to N 2 Protect and connect the tail gas absorption device; take 9.34g (0.046mol) of phthaloyl chloride and dissolve it in 60ml NMP and place it in a constant pressure dropping funnel, drop the phthaloyl chloride solution at a speed of 1-2 drops / s Add in the piperazine solution, the temperature of the system is controlled at 25 ° C, and the reaction is continued for 0.5 h after the dropwise addition to obtain the solution of the prepolymer A2; ) Tripiperazine-triazine was dissolved in 20ml of NMP and placed in a constant pressure dropping funnel. After the prepolymer was dissolved, the triperazine-triazine solution w...
Embodiment 3
[0050] Embodiment 3: step (1)-step (3) is the same as embodiment 1; wherein, the preparation of step (4) prepolymer A2: take 2.16g (0.02mol) of p-phenylenediamine and add 40ml NMP solution at 20°C Add the acid binding agent triethylamine 1.01g (0.01mol) and 4g CaCl at the same time 2 Stir in the three-necked flask at a speed of 300 r / min until uniform, and the system is connected to N 2 Protect and connect the tail gas absorption device; take 5.07g (0.025mol) of isophthaloyl chloride and dissolve it in 40ml NMP and place it in a constant pressure dropping funnel, drop the isophthaloyl chloride solution at a speed of 1-2 drops / s Add in the piperazine solution, the temperature of the system is controlled at 40 ° C, and the reaction is continued for 1 h after the dropwise addition to obtain the solution of the prepolymer A2; Step (5) Preparation of macromolecular char-forming agent: take 1.33g (0.004mol) Tripiperazine-triazine was dissolved in 20 ml of NMP and placed in a const...
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