Method for improving quality of industrial N-methylpyrrolidone

A technology for methyl pyrrolidone and methyl pyrrolidone is applied in the field of improving the quality of industrial grade N-methyl pyrrolidone, can solve the problems of high risk, difficult process control and high input cost, and achieves convenient operation process, stable product quality and high cost low cost effect

Inactive Publication Date: 2011-04-06
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has high input costs, high energy consumption, difficult process control, high risk, and it is difficult to obtain products that meet the requirements of high-purity N-methylpyrrolidone for large-scale industrial production

Method used

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  • Method for improving quality of industrial N-methylpyrrolidone
  • Method for improving quality of industrial N-methylpyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: Pretreatment of macroporous adsorption resin, strongly acidic cation exchange resin and strongly basic anion exchange resin.

[0024] 1) Pretreatment of macroporous adsorption resin: use organic alcohol solvents (such as ethanol, isopropanol, etc.) to soak and rinse the adsorption resin until the organic alcohol at the rinse outlet of the resin does not become turbid after adding water, and then use high-purity Ionized water rinses the adsorbent resin until the TOC of the rinsed water is less than 5.

[0025] 2) Pretreatment of strongly acidic cation exchange resin: after transforming the cation exchange resin into H-type, wash the cation exchange resin with high-purity water until the conductivity of the resin washing water is 1-10 μS / cm.

[0026] 3) Pre-treatment of strongly basic anion exchange resin: After transforming the anion exchange resin into OH type, wash the anion exchange resin with high-purity water until the conductivity of the resin washing water...

Embodiment 2

[0032] The macroporous adsorption resin, strongly acidic cation exchange resin and strongly basic anion exchange resin were pretreated, and the adsorption resin was soaked and rinsed with organic alcohol solvent isopropanol, and the rest of the steps were the same as in Example 1.

[0033] The standard and analysis result of table 1N-methylpyrrolidone

[0034] project

unit

SEMI C8 standard

Example 1

Example 2

NMP content

wt%

99.80

99.82

99.89

Exterior

APHA

≤30

15

17

Water content (H 2 O)

％

≤0.03

0.015

0.013

Free amine (as CH 3 NH 2 )

ppm

≤5

3

3

Chloride (Cl)

ppb

≤300

119

117

Nitrate (NO 3 )

ppb

≤400

230

255

Phosphate (PO 4 )

ppb

≤250

111

114

Sulfate (SO 4 )

ppb

≤250

125

122

Aluminum (Al)

ppb

≤5

0.02

0.02

Ant...

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Abstract

The invention discloses a method for improving the quality of industrial N-methylpyrrolidone, comprising the following steps of: taking industrial N-methylpyrrolidone as a raw material, orderly removing amine, cation and anion impurities in the industrial N-methylpyrrolidone with a macroporous absorbent resin column, a strong-acid cation exchange resin column and a strong-base anion exchange resin column which are connected in series to form an ion exchange device, and then rectifying and filtering with a membrane to obtain N-methylpyrrolidone with improved quality. Analysis and detection show that the free amine content (based on methylamine) of the product is smaller than 5ppm, and both the anion impurity content and the cation impurity content meet the requirements on SEMI-C8 standards of chemical material part, established by the Semiconduct or Equipment and Materials International. The ion exchange resin used in the method can be regenerated and reclaimed, has the advantage of low carbon and is environment-friendly. The operation process is simple, and product quality is stable. The method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for improving the quality of industrial-grade N-methylpyrrolidone, in particular to a method for improving the quality of industrial-grade N-methylpyrrolidone and removing amine, cation and anion impurities therein. Background technique [0002] N-Methylpyrrolidone (NMP) is an important chemical raw material. It is a polar solvent with strong selectivity and good stability. It has high boiling point, non-flammability, low toxicity, safe use, strong solvency and recyclability. , Biodegradable and other advantages. It is mainly used for extraction agents such as butadiene and aromatic hydrocarbons, solvents for many engineering plastics (such as polyvinylidene fluoride, etc.), electrode auxiliary materials for lithium-ion batteries, photoresist removers, LCD liquid crystal material production, semiconductor industry Circuit board cleaning, etc. [0003] In the prior art, both patent WO03 / 053924A1 and patent CN1871213A ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
Inventor 沈哲瑜魏永明宋振许振良
Owner SHANGHAI CHEM REAGENT RES INST
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