Extraction-rectification recovery method of N-methyl pyrrolidone in waste solvent

A technology of methyl pyrrolidone and recovery method, which is applied in the field of chemical waste solvent recovery, can solve the problems of reducing energy consumption, and achieve the effect of green process and low energy consumption

Pending Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to reduce the energy consumption of the rectification process, some researchers have done some heat integration on the rectification process, such as the patent document CN 103058909 B, but this method reduces energy consumption to a limited extent

Method used

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  • Extraction-rectification recovery method of N-methyl pyrrolidone in waste solvent
  • Extraction-rectification recovery method of N-methyl pyrrolidone in waste solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A batch of spinning waste solvent, which contains 2% N-methylpyrrolidone after determination, is injected from the upper feed port of the rotary disk sieve plate extraction tower with a flow rate of 20ml / min. With octanoic acid as the extractant, the flow rate is set at 10ml / min, and it enters from the lower feeding port of the rotary disk sieve plate extraction tower. The speed of the turntable was set at 10 r / min, the extraction temperature was 25° C., and the extraction phase was obtained at the top of the extraction tower. The extraction phase enters from the middle of the rectification tower, the pressure is set to 0.75atm, the reflux ratio is set to 1, the temperature at the top of the tower is controlled at 190.8°C, and the top fraction at this temperature is collected. Finally, the obtained overhead fraction is sequentially passed through the decolorization tower and the dehydration tower to finally obtain the N-methylpyrrolidone product. The N-methylpyrrolidone...

Embodiment 2

[0030]A batch of spinning waste solvent, which contains 5% N-methylpyrrolidone after determination, is injected from the upper feed port of the rotary disk sieve plate extraction tower with a flow rate of 20ml / min. With octanoic acid as the extractant, the flow rate is set at 20ml / min, and it enters from the lower feeding port of the rotary disk sieve plate extraction tower. The speed of the turntable was set at 20 r / min, the extraction temperature was 25° C., and the extraction phase was obtained at the top of the extraction tower. The extraction phase enters from the middle of the rectification tower, the pressure is set to 0.75atm, the reflux ratio is set to 1, the temperature at the top of the tower is controlled at 190.8°C, and the top fraction at this temperature is collected. Finally, the obtained overhead fraction is sequentially passed through the decolorization tower and the dehydration tower to finally obtain the N-methylpyrrolidone product. The N-methylpyrrolidone ...

Embodiment 3

[0032] A batch of spinning waste solvent, which contains 20% N-methylpyrrolidone after determination, is injected from the upper feed port of the rotary disk sieve plate extraction tower with a flow rate of 20ml / min. With octanoic acid as extractant, the flow rate is set as 40ml / min, and enters from the lower feed port of the rotary disk sieve plate extraction tower. The speed of the turntable was set at 40 r / min, the extraction temperature was 25° C., and the extraction phase was obtained at the top of the extraction tower. The extraction phase enters from the middle of the rectification tower, the pressure is set to 0.75atm, the reflux ratio is set to 1, the temperature at the top of the tower is controlled at 190.8°C, and the top fraction at this temperature is collected. Finally, the obtained overhead fraction is sequentially passed through the decolorization tower and the dehydration tower to finally obtain the N-methylpyrrolidone product. The N-methylpyrrolidone has a pu...

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Abstract

The invention provides an extraction-rectification recovery method of N-methyl pyrrolidone. The N-methyl pyrrolidone is recycled by taking a selected solvent or a composite solvent as an extracting agent and an extraction-rectification technology as a core, and the method specifically comprises the following steps: firstly, extracting by using the extracting agent, rectifying an obtained extractedphase to respectively recycle the N-methyl pyrrolidone and the extracting agent, and refining the N-methyl pyrrolidone to finally obtain a product. According to the method, the extraction efficiencyof the selected extracting agent is high, the process technology is green, simple and convenient, the operability is high, the purity of the obtained N-methyl pyrrolidone is larger than 99.7%, the moisture content is lower than 200 ppm, the recovery rate is 97% or above, compared with other technological methods, the process energy consumption is remarkably reduced, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the field of recovery of chemical waste solvents, in particular to an N-methylpyrrolidone recovery process using a selected solvent or a composite solvent as an extraction agent and taking extraction-rectification as the core separation and recovery method. Background technique [0002] N-Methyl pyrrolidone (N-Methyl pyrrolidone, NMP), also known as 1-methyl-2-pyrrolidone, is an important petrochemical solvent. At room temperature, it is a colorless to pale yellow transparent liquid with a slight ammonia odor, strong hygroscopicity, stable chemical properties and low viscosity. In addition, N-methylpyrrolidone has the advantages of good chemical and thermal stability, high polarity, low volatility, and infinite miscibility with water and many organic solvents. These advantages make it widely used in many fields. For example, it is often used as an extraction agent in syngas desulfurization and lubricating oil refining. It also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 秦磊蔡立鑫陈亮
Owner CHINA PETROLEUM & CHEM CORP
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