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A kind of piperazine composite ionic liquid, its preparation method and its application in dissolving aramid fiber 1313

A technology of composite ions and ionic liquids, which is applied in the field of preparation of piperazine composite ionic liquids, can solve the problems of catalytic degradation and dissolution of aramid fibers that have not been reported in ionic liquids, and achieve easy large-scale preparation, good stability, and stable properties Effect

Active Publication Date: 2021-07-23
浙江蓝德能源科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the application of ionic liquids in catalytic degradation and dissolution of aramid fiber 1313

Method used

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  • A kind of piperazine composite ionic liquid, its preparation method and its application in dissolving aramid fiber 1313
  • A kind of piperazine composite ionic liquid, its preparation method and its application in dissolving aramid fiber 1313

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Example 1: Preparation of 1-ethyl-4-methylpiperazine chloride salt and 1-butyl-4-methylpiperazine bisulfate composite (1:1) ionic liquid

[0047]Synthesis of 1-ethyl-4-methylpiperazine chloride salt: take a sealed reaction kettle lined with polytetrafluoroethylene liner, add 2.0mol of 1-chloroethane, 200ml of toluene and 1.0mol of N-methylpiperazine Add magnetrons, magnetically stir, seal the reaction kettle, transfer to a constant temperature magnetic stirrer, stir and react at 80°C for 48h, after the reaction is completed, cool to room temperature, filter to remove the toluene in the solution and the impurities contained therein, and obtain The crude product was washed with n-heptane, using 100ml each time, and washed 3 times. After filtration and vacuum drying at 50°C, 1-ethyl-4-methylpiperazine chloride salt was obtained with a purity of 98% and a yield of 93%.

[0048] Synthesis of 1-butyl-4-methylpiperazine hydrogen sulfate: take a sealed reactor lined with polyt...

Embodiment 2

[0050] Example 2: Preparation of 1-propyl-4-methylpiperazine chloride salt and 1-hexyl-4-methylpiperazine bisulfate composite (1:2) ionic liquid

[0051] Synthesis of 1-propyl-4-methylpiperazine chloride salt: except that 2.0 mol of 1-chloroethane was replaced by 1.5 mol of 1-chloropropane, and reacted at 100°C for 24 hours, the rest were the same as in Example 1 Synthesis of 4-methylpiperazine chloride salt. Under these conditions, 1-propyl-4-methylpiperazine chloride salt was obtained with a purity of 95% and a yield of 90%.

[0052] Synthesis of 1-hexyl-4-methylpiperazine hydrogen sulfate: except that 1-chlorobutane is replaced by 1-chlorohexane, and the reaction time is 72h, the rest are the same as 1-butyl-4-methyl in Example 1 Synthesis of piperazine bisulfate. Under these conditions, 1-hexyl-4-methylpiperazine hydrogen sulfate was obtained with a purity of 95% and a yield of 88%.

[0053] Preparation of composite ionic liquid: except that the molar ratio is 1:2, othe...

Embodiment 3

[0055] Preparation of 1-hexyl-4-methylpiperazine chloride salt and 1-butyl-4-methylpiperazine p-toluenesulfonate composite (1:3) ionic liquid 1-hexyl-4-methylpiperazine Chloride salt synthesis: except that 2.0 mol of 1-chloroethane was replaced by 3.0 mol of 1-chlorohexane, and reacted at 130°C for 72 hours, the rest were the same as the 1-ethyl-4-methylpiperazine chloride salt in Example 1 synthesis. Under these conditions, 1-hexyl-4-methylpiperazine chloride salt was obtained with a purity of 96% and a yield of 94%.

[0056] Synthesis of 1-butyl-4-methylpiperazine p-toluenesulfonate: except that 100g of concentrated sulfuric acid was replaced by 172.2g of p-toluenesulfonic acid, and reacted at 100°C for 60h, the rest was the same as that of 1-butyl-4 in Example 1 - Synthetic synthesis of methylpiperazine bisulfate. Under these conditions, 1-butyl-4-methylpiperazine p-toluenesulfonate was obtained with a purity of 97% and a yield of 96%.

[0057] Preparation of composite i...

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Abstract

The invention belongs to the field of synthesis and application of ionic liquids, and in particular relates to a preparation method of a piperazine compound ionic liquid, and its application to catalytic degradation and dissolution of aramid fiber 1313. The preparation method comprises the following steps: Step 1: chloroalkane ( R 1 Cl) and N-methylpiperazine react in toluene solution to obtain the formula I ionic liquid; Step 2: chloroalkane (R 2 Cl) and N-methylpiperazine react in a toluene solution, then filter (the product is a solid) or liquid separation (the product is a liquid), after concentration, add HY (anionic acid) at room temperature, complete the reaction, and dry Finally, the ionic liquid of formula II is obtained; step 3: after mixing the ionic liquids of formula I and formula II, the temperature is raised and stirred, and the compound ionic liquid is obtained after drying.

Description

technical field [0001] The invention belongs to the field of synthesis and application of ionic liquids, and in particular relates to a preparation method of a piperazine compound ionic liquid and its application to catalytic degradation and dissolution of aramid fiber 1313. Background technique [0002] Aramid 1313 is called polym-phenylene isophthalamide fiber, which is a kind of polyamide fiber. It is a kind of aramid fiber. [0003] The full name of aramid fiber is "aromatic polyamide fiber", which is a new type of special polymer fiber with good or excellent mechanical properties, flame retardancy, heat resistance, stable chemical properties, radiation resistance, friction resistance, etc. Used in various fields, such as brake pads, gaskets, optical fiber protection, high temperature filter bags, automotive hoses, tires, power transmission belts, rubber shoe soles, cut-resistant gloves, etc. At present, the global aramid production capacity is about 150,000 tons. Ara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/037B01J31/02B09B3/00
CPCB01J31/0282B09B3/00C07D295/037
Inventor 任旭华沈珏峰
Owner 浙江蓝德能源科技发展有限公司
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