Synthesis of methyl carbamate and dimethyl carbonate (DMC) in presence of stripping with inert gas or superheated vapours and a reactor for the same

Patent metadata

Field	Value
Publication number	US-9920000-B2
Application number	US-201314441753-A
Country	US
Kind code	B2
Filing date	Nov 11, 2013
Priority date	Nov 9, 2012
Publication date	Mar 20, 2018
Grant date	Mar 20, 2018

Abstract

The invention relates to synthesis of methyl carbamate (MC) and dimethyl carabonate (DMC) in presence of stripping inert gas or superheated methanol vapors using packed column reactor and bubble column reactor.

First claim

The invention claimed is:

1. A process for synthesis of methyl carbamate and dimethyl carbonate (DMC) in a reactor, the process comprising:
a. feeding a liquid reactant feed comprising urea and methanol or methyl carbamate and methanol into a reactor vessel containing a catalyst, wherein the catalyst is either a heterogeneous catalyst in a form of an expanded slurry bed of solid catalyst particles suspended in a suspension liquid or in a packed bed of solid catalyst, or a homogenous catalyst, wherein the homogenous catalyst is a samarium nitrate catalyst dissolved in the liquid reactant feed present in the reactor, and allowing the liquid reactant feed and the catalyst to react in the reactor vessel;
b. passing inert gas or superheated methanol vapours into the reactor vessel through an inlet valve by regulating a pressure to ensure positive flow of the inert gas or superheated methanol vapours, and stripping ammonia and DMC formed during a reaction in the reactor vessel through an outlet port;
c. passing the ammonia and DMC collected from the outlet port through a condenser and a gas-liquid separator;
d. removing liquid phase products from the reactor vessel through a liquid outlet post; and
e. recycling a stream of methanol or gaseous product leaving the gas-liquid separator into the reactor vessel for further reaction, through an inlet port.

2. The process according to claim 1 , wherein the reactor used is selected from packed bed reactors and bubble column reactors having counter-current and cross-current stripping.

3. The process according to claim 1 , wherein the catalyst is a heterogeneous catalyst selected from the group consisting of hydrotalcite, double metal cyanides, and cenospheres.

4. The process according to claim 1 , wherein a concentration of the catalyst particles present in the slurry bed is in a range of 0.01 to 10 weight percentage.

5. The process according to claim 1 , wherein the inert gas is selected from air, CO 2 , He, Ar, and N 2 .

6. The process according to claim 1 , wherein a velocity of the inert gas or superheated methanol vapors used for stripping the ammonia and DMC is in a range of 1×10 −4 to 0.1 m/s.

7. The process according to claim 1 , wherein the pressure in step (b) is regulated by maintaining a constant pressure difference between a constant pressure regulator fitted to the inlet valve and a back pressure regulator fitted to the outlet port to ensure positive flow of the inert gas.

8. The process according to claim 1 , wherein the reactor is maintained at a temperature in a range of 130-210° C.

9. The process according to claim 1 , wherein the process is batch or continuous.

10. The process according to claim 1 , wherein a ratio by weight of the stream of the methanol or gaseous product leaving the gas-liquid separator and recycled into the reactor vessel to the liquid reactant feed is in a range of 0.5 to 15.

11. The process according to claim 1 , wherein the reactor is a bubble column reactor selected from horizontal bubble column and horizontal sectionalized bubble column reactors.

Assignees

• Council Scient Ind Res

Inventors

• Ranade Vivek Vinayak
• Kelkar Ashutosh Anant
• Rane Vilas Hari
• Kinage Anil Kisan
• Shingote Savita Kiran
• Roy Lalita Sanjib

Classifications

• C07C269/00 Primary

  Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups [IMAGE cpc-sch-C07C-0964.gif], the nitrogen atom not being part of nitro or nitroso groups · CPC title

• B01J2219/182

  horizontal · CPC title

• B01J2219/00006

  Large-scale industrial plants · CPC title

• Y02P20/582

  Recycling of unreacted starting or intermediate materials · CPC title

• B01J2208/00123

  Fingers · CPC title