8/26/2017 Patent CN101508667A - Purification method of N-methyl pyrrolidone - Google Patenten

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Purification method of N-methyl pyrrolidone Publicatienummer CN101508667 A

CN 101508667 A Publicatietype Aanvraag
Aanvraagnummer CN 200910064504
Publicatiedatum 19 aug 2009
SAMENVATTING
Aanvraagdatum 30 maart 2009
Prioriteitsdatum 30 maart 2009
The invention relates to a method for purifying N-methylpyrrolidone, which is a
method for producing a heterocyclic compound. The method comprises the Uitvinders 宋国全, 理 杨, 强 肖

following steps: adding a water repellent agent accounting for 0.1 to 2 percent Aanvrager 濮阳迈奇科技有限公司
of a crude product into crude product solution, and then continuously throwing Citatie exporteren BiBTeX, EndNote, RefMan
the mixture into a three-tower combined rectifying system. By adopting good- Verwijzingen naar dit patent (9), Classificaties (2),
quality stuffing and three-tower continuous pressure reduced rectification, Juridische gebeurtenissen (3)
adopting an advanced rectifying operation method according to the optimal Externe links: SIPO, Espacenet
principle of reflux separation effect, and adopting a reflux ratio of 1.5 to 3 to
extract a product, the method effectively controls the contents of impurities such
as metal ions and the like.

BESCHRIJVING vertaald uit het Chinees CLAIMS (4) vertaald uit het Chinees

One kind of method for purifying N- methylpyrrolidone
First, the present invention relates to a method for producing a heterocyclic
compound, in particular a method for purifying methyl ketone embankment
pyrrole N-.
II BACKGROUND ART: The traditional method for purifying N- methyl
pyrrolidone, the desired product N
A lower purity and yield methylpyrrolidone, high moisture, impurities.
III. SUMMARY: The purpose of the present invention is to provide a high quality
product, low moisture content, and the quality and stability of a kind suitable for
industrial production method for purifying methylpyrrolidone N-. It solves the
problems of other technologies, an object of the invention is achieved, it is the
1. A method for purifying N- methylpyrrolidone, wherein: the water-blocking
agent by 0.1-2% crude was added to the crude solution and then was
successively into the three towers combined distillation system, using high-
quality filler , three-tower continuous vacuum distillation, pressure control at -80
to -95kPa, using advanced methods of operation in accordance with reflux
distillation optimal separation principle, the use of a reflux ratio of 1.5-3 mined
products, effective control of the metal ion content of other impurities, purity
≥99.9%, moisture content ≤100ppm, N- methylpyrrolidone yield above 99%.
2, wherein a method for purifying a ketone of N- methylpyrrolidine
embankment claim, characterized in that: said water-blocking agent is
a strong base weak acid salt.
3, the 1 A method for purifying N- methylpyrrole embankment one of

water cut-off the preceding claims, characterized in that: after the three towers of
the production method according to the combination of the distillation
Agent strong base weak acid salt by 0.1-2% crude solution was added to the system, i.e., stripped off the column amine amine, fed to the
crude solution and then was successively hit dehydration Tower of dehydration, the material enters the product after
dehydration tower taken directly to products, the entire process of
The deamination tower, dehydration towers, three towers combined product
continuous production.
column distillation system, using high-quality filler, Three Pagodas
4, the 1 A method for purifying N- methylpyrrolidone claim,
Continuous vacuum distillation, pressure control at -80 to -95kPa, using
characterized in that: based on the principle of optimal separation
advanced methods of operation in accordance with reflux distillation optimal
reflux, a reflux ratio of 1.5-3 product recovery method.
separation principle, the use of a reflux ratio of 1.5-3 mined products, effective
control of the metal ions and other impurities The content, improved product
yield and purity.

The production method of the present invention, since the crude was added water blocking agent, while the use of
advanced methods of operation fine leavened effectively reduced moisture content of the product, improve product purity
and yield. The purification method advanced technology and reasonable, easy to operate, low production costs. The
purification process of the present invention provides the production of N- methylpyrrolidone is an important chemical raw
materials, is a good selectivity and stability of the polar solvents with low toxicity, high boiling point, dissolution and strong,
non-flammable, can biodegradable, recyclable, safe and suitable for use in a variety of formulations and so on. Which is
mainly used for acetylene and concentrate butadiene, isoprene, aromatics extraction, refining lubricating oil, insoluble
plastic (polyphenylene sulfide, polyimide) and the polymerization solvent aramid fiber, electronic insulation material,
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8/26/2017 Patent CN101508667A - Purification method of N-methyl pyrrolidone - Google Patenten
lithium-ion batteries, high-grade paint, ink, paint, pesticide chemicals, cleaning agents: de-oiling, degreasing, dewaxing,
polished, rust, peeling paint, artificial kidney function film liquid, desalination film liquid. Its structural formula is:

<Formula> formula see original document page 4 </ formula>

Purity "99.9%, moisture content" 100ppm, yield 99%.

Fourth, the specific embodiments: This invention is a water-blocking agent is a strong base weak acid salt of 0.1 to 2%
crude solution was added to the crude solution and then was successively into deamination tower, dehydration towers,
three towers tower product portfolio distillation system, using high-quality packing, three-tower continuous vacuum
distillation, pressure control at -80 to -95kPa, using advanced methods of operation in accordance with reflux distillation
optimal separation principle, the use of a reflux ratio of 1.5-3 products recovery, effective control of the content of the metal
ions and other impurities, improved product yield and purity; effective control of the content of the metal ions and other
impurities, product purity "of 99.9% moisture content" 100ppm, N- methylpyrrolidone The yield of over 99%.

VERWIJZINGEN NAAR DIT PATENT

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* Geciteerd door patentambtenaar

CLASSIFICATIES

Internationale classificatie B01D3/10, C07D207/267

JURIDISCHE GEBEURTENISSEN
Datum Code Gebeurtenis Beschrijving
19 aug 2009 C06 Publication
14 okt 2009 C10 Request of examination as to substance
14 sept 2011 C12 Rejection of an application for a patent

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