Configuration and its use in process for synthesis of alkyl carbamates from alkyl alcohol and urea in a tubular reactor

Patent metadata

Field	Value
Publication number	US-10487048-B2
Application number	US-201615558072-A
Country	US
Kind code	B2
Filing date	Mar 11, 2016
Priority date	Mar 13, 2015
Publication date	Nov 26, 2019
Grant date	Nov 26, 2019

Abstract

The present invention discloses an improved catalyst free process for synthesis of alkyl carbamates in an integrated system comprising a tubular reactor and a striper. The process comprises reacting urea and an alcohol in said tubular reactor under autogeneous pressure; wherein said process provides >90% selectivity towards alkyl carbamate. The mixture of urea and alcohol is N fed to the tubular reactor at a particular feed rate. The tubular reactor is heated externally under autogeneous pressure to carry out a synthesis reaction producing alkyl carbamate and ammonia. The ammonia is removed from the tubular reactor by the striper. The tubular reactor and the stripper are arranged in series to reduce the equilibrium limitations of the reaction and drive the reaction in forward direction.

First claim

The invention claimed is:

1. A catalyst free process for synthesis of alkyl carbamate within an integrated system of at least one tubular reactor and a stripper in series, comprising: (1) reacting urea and an alcohol in said tubular reactor under autogenous pressure, (2) pumping the mixture of step (1) into a tubular reactor with a pump at a feed rate in the range of 2-25 ml/min; and (3) maintaining the pressure of the reactor of step (2) using a back pressure regulator mounted downstream from the tubular reactor and collecting the desired carbamate, wherein said process provides >90% selectivity towards alkyl carbamate, wherein the alcohol is selected from methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, tert-butanol, pentanol, and hexanol.

2. The catalyst free process according to claim 1 , wherein the temperature of the reaction mixture is in the range of 150-250° C.

3. The catalyst free process according to claim 1 , wherein urea and alcohol in mole ratio 10 to 50 are fed in to the tubular reactor at a feed rate of 5-25 ml/min and a residence time less than 1 hour.

4. The catalyst free process according to claim 1 , wherein said process can be carried out continuously, semi continuously or batch wise.

5. The catalyst free process according to claim 1 , wherein the process further comprises reacting said alkyl carbamate with an alcohol to obtain dialkyl carbonate in said integrated system.

6. An integrated system for a catalyst free process for the synthesis of alkyl carbamate as claimed in claim 1 comprising at least one tubular reactor, heated externally, for reacting urea and alcohol and a stripper for removal of ammonia formed during the said process, wherein said tubular reactor and said stripper are arranged in series to reduce the equilibrium limitations of the reaction and drive the reaction in forward direction.

7. The integrated system according to claim 6 , further comprises DMC reactor, wherein said alkyl carbamate obtained is reacted with alcohol vapors to obtain dialkyl carbonates.

8. The integrated system according to claim 6 , wherein the diameter of the tubular reactors is ½″ and the length is in the range of 4 to 9 meters to achieve adequate residence time and high conversion rate of urea.

9. The integrated system according to claim 6 , wherein the temperature of the tubular reactor is in the range 150-250° C.

Assignees

• Council Scient Ind Res

Inventors

• Ranade Vivek Vinayak
• Kelkar Ashutosh Anant
• Rane Vilas Hari
• Kinage Anil Kisan
• Mote Dhananjay Ravindra
• 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

• B01J2219/00033

  Continuous processes · CPC title

• C07C271/12

  to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals · CPC title

• C07C68/00

  Preparation of esters of carbonic or haloformic acids · CPC title

• C07C69/96

  Esters of carbonic or haloformic acids · CPC title