Title of Invention | A PROCESS TO MANUFACTURE N-METHYL-2-PYRROLIDONE (=1-METHYL-2-PYRROLIDONE,NMP) |
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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: l 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). 2 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 3 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%. 4 |
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04-mum-2007-correspondence-received.pdf
04-mum-2007-description (provisional).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 | |||||||||
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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:
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PCT International Classification Number | C07D207/00 | |||||||||
PCT International Application Number | N/A | |||||||||
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PCT Conventions:
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