Title of Invention

A PROCESS TO MANUFACTURE N-METHYL-2-PYRROLIDONE (=1-METHYL-2-PYRROLIDONE,NMP)

Abstract This invention relates to a process to Manufacture N-Methyl-2-Pyrrolidone (=1-Methyl-2-pyrrolidone, NMP) by reaction of Gamma Butyrolactone ([gamma]-BL) with mono Methylamine (MMA) at a temperature of 200°-300°C and at a pressure of 25-100 kg/cm gauge and molar ratio of 1:1, 1-1.5.
Full Text FORM NO 2
THE PATENTS ACT, 1970.
(39 OF 1970)
PROVISIONAL SPECIFICATION [See sections 10 and Rule 13]
TITLE A Process to Manufacture N-Methyl-2-
Pyrrolidone (=l-Methyl-2-Pyrrolidone,
NMP).
APPLICANT BALAJI AMINES LIMITED
ADDRESS 165/A, Balaji Bhavan, Railway Lines, Solapur
413 001.
NATIONALITY Indian
The following specification describes the nature of this invention and the manner in which it is to be performed:
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TITLE
A Process to Manufacture N-Methyl-2-Pyrrolidone (=l-Methyl-2-Pyrrolidone, NMP).
FIELD OF THE INVENTION
This invention relates to a process to Manufacture N-Methyl-2-Pyrrolidone (=l-Methyl-2-Pyrrolidone, NMP) by reaction of Gamma Butyrolactone ([gamma]-BL) with Mono Methylamine (MMA) at a temperature of 200° -300°C and at a pressure of 25-100 kg /cm gauge and molar ratio of 1 : 1.1-1.5
BACKGROUND OF THE INVENTION
The industrial preparation of NMP is predominantly carried out by reaction of gamma-Butyrolactone ([gamma]-BL) with Mono Methylamine (MMA) in a tubular reactor, e.g. a shaft reactor, at from 200 to 350[deg.] C. and super atmospheric pressure, e.g. about 10 MPa (Ullmann's Encyclopedia of Industrial Chemistry, 5th edition., Vol. A22, pages 458 to 459 (1993))
Also, there are several processes for the synthesis of NMP from gamma-
Butyrolactone ([gamma]-BL) with Mono Methylamine (MMA) as a starting
material. In several patents (JP 7 221 420; JP 7400259; JP 7 420 585;
JP 7 642 107) Mitsubishi Chemical Industries Co. Ltd. of Japan
described continuous processes for the synthesis of NMP using GBL and
MMA as starting materials. These are characterised by reactions with
high molar ratios between water and shot GBL (typically ranging between
3 and 4 mols of water for each mol of GBL) and by the presence of great
amounts of MMA (typically with molar ratios ranging between 1.4 and 3
moles of MMA per mol of GBL).
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The processes described by Mitsubishi amount to be disadvantageous in terms of the high costs involved with the separation of excess MMA
and its recovery and with the separation of the water forwarded to the
reaction to which synthesis water adds up (one mol of water for each mol
of reacted GBL).
To avoid the drawbacks associated with the continuous reaction in the presence of excess MMA and water, alternative methodologies have been proposed and these are based on the employment of catalysts.
The present invention is an attempt to develop a process for manufacturing NMP with out any catalyst and to obtain high yield and purity of NMP with a low investment cost.
OBJECT OF THE INVENTION
The object of the invention is to manufacture NMP by reacting MMA and GBL without the use of any catalysts. The other object of invention is the production of NMP at low investment cost and low utility consumption.
Also, the object of the invention is to see that the reaction takes place in a continuous fashion with low molar ratio between GBL and MMA , i.e., 1: 1.1-1.5
DESCRIPTION OF THE INVENTION
The process of the present invention is as follows:
Gamma Butyro Lactone and Mono Methyl Amine are fed to the Reactor at
the desired Molar ratio through a Mixer where intimate mixing of the two
takes place before entering the first of the three reactors. The reaction
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between GBL and MMA is highly exothermic and the temperature after mixing reaches 150 - 175 Deg.C.
The reaction mixture then passes to the first reactor where the temperature is raised to 200-220 Deg.C by external heating. The reaction mixture from the reactor then passes to a second reactor where it is further heated to a temperature of 230 - 250 Deg.C. The reaction mixture is then passed to a third reactor where it is further raised to 270 - 300 Deg.C. at which temperature the reaction goes to completion. All the reactors are sized to attain the desired residence times for the forward reaction to proceed.
Pressure of the reactors is maintained by a Pressure controlling device. Reaction mixture from the pressure control device is sent to a flash vessel where excess MMA is vented and absorbed in water and sent to Methyl Amines plant for recovery. Liquid containing NMP, unreacted GBL and water are fed to a water removal column followed by an NMP
recovery column, both of which are operated under vacuum. NMP thus obtained has a purity of not less than 99.7% and in a yield of greater
than 90%.

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Documents:

04-mum-2007-correspondence-received.pdf

04-mum-2007-description (provisional).pdf

04-mum-2007-form-1.pdf

04-mum-2007-form-2.doc

04-mum-2007-form-2.pdf

4-MUM-2007-ABSTRACT(7-5-2014).pdf

4-MUM-2007-CLAIMS(28-3-2007).pdf

4-MUM-2007-CLAIMS(AMENDED)-(28-5-2013).pdf

4-MUM-2007-CLAIMS(AMENDED)-(7-5-2014).pdf

4-MUM-2007-CORRESPONDENCE(28-3-2007).pdf

4-MUM-2007-DESCRIPTION(COMPLETE)-(28-3-2007).pdf

4-MUM-2007-DRAWING(28-3-2007).pdf

4-MUM-2007-DRAWING(7-5-2014).pdf

4-MUM-2007-FORM 1(28-5-2013).pdf

4-MUM-2007-FORM 18(28-5-2010).pdf

4-MUM-2007-FORM 2(COMPLETE)-(28-3-2007).pdf

4-MUM-2007-FORM 2(TITLE PAGE)-(7-5-2014).pdf

4-MUM-2007-FORM 2(TITLE PAGE)-(COMPLETE)-(28-3-2007).pdf

4-MUM-2007-FORM 2(TITLE PAGE)-(PROVISIONAL)-(2-1-2007).pdf

4-MUM-2007-FORM 26(28-5-2013).pdf

4-MUM-2007-FORM 3(28-5-2013).pdf

4-MUM-2007-FORM 5(28-5-2013).pdf

4-MUM-2007-PETITION UNDER RULE-137(7-5-2014).pdf

4-MUM-2007-REPLY TO EXAMINATION REPORT(28-5-2013).pdf

4-MUM-2007-REPLY TO HEARING(7-5-2014).pdf

4-MUM-2007-SPECIFICATION(AMENDED)-(7-5-2014).pdf


Patent Number 260810
Indian Patent Application Number 4/MUM/2007
PG Journal Number 21/2014
Publication Date 23-May-2014
Grant Date 22-May-2014
Date of Filing 02-Jan-2007
Name of Patentee BALAJI AMINES LIMITED
Applicant Address 165/A, BALAJI BHAVAN, RAILWAY LINES, SOLAPUR
Inventors:
# Inventor's Name Inventor's Address
1 VATTEM RAMA CHANDRA 165/A, BALAJI BHAVAN, RAILWAY LINES, SOLAPUR-413001
2 SHAM RAO NA165/A, BALAJI BHAVAN, RAILWAY LINES, SOLAPUR-413001
PCT International Classification Number C07D207/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA