Method for preparing biuret polyisocyanate

Patent metadata

Field	Value
Publication number	US-9701624-B2
Application number	US-201415104338-A
Country	US
Kind code	B2
Filing date	Apr 15, 2014
Priority date	Dec 20, 2013
Publication date	Jul 11, 2017
Grant date	Jul 11, 2017

Abstract

A method for continuously preparing biuret polyisocyanate, comprising: a mixed solution of a diisocyanate and a catalyst with water vapour, in an aerosol form, are continuously reacted in a first reactor; the product obtained therefrom is brought into a second reactor for a further reaction; a tail gas from the second reactor is condensed and refluxed, and the non-condensable gas is brought into a tail gas treatment system; a reaction liquid obtained in the second reactor is further reacted in a third reactor; and then separation is performed for removing monomers, so as to obtain biuret polyisocyanate.

First claim

The invention claimed is:

1. A method for continuously preparing biuret polyisocyanate, comprising the following steps:
a) a mixed solution of a diisocyanate and a catalyst, and water vapour, in an aerosol form, are continuously reacted in a first reactor; wherein the continuous phase of the aerosol is the water vapour, the dispersed phase is the mixed solution of the diisocyanate and the catalyst, and the droplet size of the dispersed phase in the aerosol in step a) is 0.01-50 μm;
b) the product obtained in step a) is brought into a second reactor for a further reaction; a tail gas from the second reactor is condensed and refluxed, and the non-condensable gas is brought into a tail gas treatment system;
c) the reaction liquid obtained in step b) is further reacted in a third reactor; and
d) a separation of the reaction liquid obtained in step c) is performed for removing monomers, so as to obtain biuret polyisocyanate.

2. The method according to claim 1 , characterized in that: the conversion rate of water vapour in the first reactor is 80-95%, based on the water vapour enter into the first reactor.

3. The method according to claim 2 , characterized in that: the total conversion rate of water vapour after step b) is higher than 95%, based on the water vapour enter into the first reactor.

4. The method according to claim 2 , characterized in that: the residence time of the aerosol in the first reactor in step a) is 10-60 min.

5. The method according to claim 1 , characterized in that: the absolute pressure in the first reactor in step a) is 0.1-1 Mpa, and the temperature is 100-160° C.

6. The method according to claim 1 , characterized in that: the molar ratio of diisocyanate and water vapour in step a) is 3:1-15:1.

7. The method according to claim 1 , characterized in that: said diisocyanate is one or more of aliphatic diisocyanates, alicyclic diisocyanates and aromatic diisocyanates; said catalyst is a Brnsted acid, and the amount of the catalyst is 0.1-3.0 wt % based on the total amount of diisocyanates.

8. The method according to claim 1 , characterized in that: the first reactor is a vertical tubular reactor, a tower reactor or a tank reactor with high height-to-diameter ratio.

9. The method according to claim 1 , characterized in that: the average residence time of the reaction liquid in the second reactor in step b) is 20-200 min.

10. The method according claim 9 , characterized in that: the temperature of the second reactor in step b) is 120-160° C.

11. The method according to claim 10 , characterized in that: said second reactor is a tank reactor or a tower reactor.

12. The method according to claim 1 , characterized in that: the temperature of the third reactor in step c) is 130-180° C., and the average residence time is 20-200 min.

13. The method according claim 12 , characterized in that: said third reactor is a tubular reactor.

14. The method according to claim 1 , wherein the separation for removing monomers in step d) is to separate biuret polyisocyanates from excess diisocyanate monomers through a film evaporator and/or a short-path evaporator, and the content of diisocyanate monomers in the separated biuret polyisocyanate products is less than 0.5 wt %.

15. The method according to claim 2 , characterized in that: the conversion rate of water vapour in the first reactor is 85-92%, based on the water vapour enter into the first reactor.

16. The method according to claim 3 , characterized in that: the total conversion rate of water vapour after step b) is higher than 99%, based on the water vapour enter into the first reactor.

17. The method according to claim 4 , characterized in that: the residence time of the aerosol in the first reactor in step a) is 20-40 min.

18. The method according to claim 1 , characterized in that: the droplet size of the dispersed phase in the aerosol in step a) is 0.5-20 μm.

19. The method according to claim 6 , characterized in that: the molar ratio of diisocyanate and water vapour in step a) is 5:1-12:1.

20. The method according to claim 1 , characterized in that: said catalyst is one or mixtures of more of phosphoric acid, monoalkyl phosphates, dialkyl phosphates, monoaryl phosphates, diaryl phosphates, monocarboxylic acids and dicarboxylic acids.

Assignees

• Wanhua Chemical Group Co Ltd

Inventors

• Shi Bin
• Shang Yonghua
• Li Haijun
• Hua Weiqi
• Li Yuan
• Ma Ensen
• Wang Biao

Classifications

• C07C273/1872 Primary

  Preparation of compounds comprising a -N-C(O)-N-C(O)-N- moiety · CPC title

• C07C275/62

  Y being a nitrogen atom, e.g. biuret · CPC title