Production process for ultra-pure N-methylpyrrolidone

A technology of methylpyrrolidone and production method, applied in directions such as organic chemistry, can solve problems such as complicated preparation process, difficult process control, etc., and achieve the effects of good effect, easy operation, and avoiding unstable quality

Inactive Publication Date: 2012-04-04
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a production method of ultra-pure N-methylpyrrolidone, so as to overcome the disadvantages of complicated preparation process and difficult process control in the method of the prior art

Method used

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  • Production process for ultra-pure N-methylpyrrolidone
  • Production process for ultra-pure N-methylpyrrolidone
  • Production process for ultra-pure N-methylpyrrolidone

Examples

Experimental program
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Embodiment 1

[0026] (1) Preparation of N-methylpyrrolidone pretreatment solution:

[0027] In 500L pure quartz reactor 1 equipped with heating device, stirring device, thermometer and gas distributor, add 350kg of industrial grade N-methylpyrrolidone, control the temperature at 30±5°C, and distribute the formazan through the gas distributor under agitation. Amine gas is continuously fed into technical grade N-methylpyrrolidone at a flow rate of 5L / min (feeding ratio methylamine gas: technical grade NMP=4:1, mass ratio), and maintain this temperature for 1 hour; Methylpyrrolidone is filtered through the filter 2, and then dehydrated through a Φ400×600mm 4A molecular sieve adsorber 3 at a flow rate of 6L / min at 30-40°C to obtain N-methylpyrrolidone pretreatment liquid.

[0028] (2) the production method of N-methylpyrrolidone:

[0029] The N-methylpyrrolidone pretreatment solution is passed through the first-stage membrane filter 4 and the second-stage membrane filter 5 at a pressure of 0.5...

Embodiment 2

[0032] (1) Preparation of N-methylpyrrolidone pretreatment solution:

[0033] In a pure quartz reactor with a heating device, a stirring device, a thermometer and a gas distributor, add 350kg of industrial grade N-methylpyrrolidone, control the temperature at 35±5°C, and distribute the methylamine gas through the gas distributor under agitation. Continuously feed into industrial-grade N-methylpyrrolidone at a flow rate of 6L / min (feeding ratio methylamine gas: industrial-grade NMP=6:1, mass ratio), and maintain the temperature for 1.5 hours; At a flow rate of 6L / min, dehydrate through a Φ400×600mm 4A molecular sieve adsorber, and filter to obtain N-methylpyrrolidone pretreatment liquid.

[0034] (2) the production method of N-methylpyrrolidone:

[0035] The N-methylpyrrolidone pretreatment solution is passed through a β-cyclodextrin composite membrane with a pore size of 0.2 μm under a pressure of 0.5 MPa for the first membrane filtration, and then through a 18-crown-6 compos...

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Abstract

The invention relates to a production process for ultra-pure N-methylpyrrolidone. According to the invention, industrial grade N-methylpyrrolidone is used as a raw material and is subjected to pretreatment, 4A molecular sieve adsorption and dehydration and two times of membrane filtration respectively through a beta-cyclodextrin composite membrane and a 18-crown-6 composite membrane; an obtained filtrate undergoes vacuum rectification; collected fractions are subjected to condensation at first and to third-stage membrane filtration so as to prepare a target product. Ultra-pure N-methylpyrrolidone prepared by the process provided in the invention has a purity of more than 99.8%, water content of less than 0.03% and individual metal ion content of less than 1 ppb, being in conformity with the chemical material part class 8 (SEMI C8) established by Semiconductor Equipment and Materials International. Compared to the prior art, the invention has the advantages of stable product quality, simple operation and suitability for industrial continuous production.

Description

technical field [0001] The invention relates to a production method of ultrapure N-methylpyrrolidone, in particular to a production method of ultrapure N-methylpyrrolidone conforming to the SEMIC8 standard. Background technique [0002] N-methylpyrrolidone (N-methylpyrrolidone, referred to as NMP) belongs to the nitrogen heterocyclic compound and is an important chemical raw material, which is widely used in petrochemical, pesticide, medicine, electronic materials and other fields. Among them, electronic grade N-methylpyrrolidone In the microelectronics industry and the semiconductor industry, pyrrolidone can be used as a cleaning agent for precision instruments or circuit boards, a photoresist remover, a solvent for LCD liquid crystal material production, and an electrode auxiliary material for lithium batteries. Its purity and cleanliness It has a very important impact on the yield, electrical performance and reliability of electronic products. In recent years, due to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 詹家荣茅惠萍沈哲瑜
Owner SHANGHAI CHEM REAGENT RES INST
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