Claims
- 1. In a method wherein monoethanolamine is reacted with ethylenediamine in the presence of a phosphorus containing catalyst to provide an essentially noncyclic product comprising polyethylenepolyamines, the improvement for conducting said process on a continuous basis which comprises:
- a. using, as a catalyst, thermally activated calcined pelleted titania having thermally chemically bonded to at least the surface thereof about 0.5 to about 10 wt. % of phosphorus, said catalyst having been prepared by treating titania pellets with polyphosphoric acid for a period of time ranging from about 0.5 to about 5 hours, and thereafter water washing, recovering and drying the thus-treated pellets,
- b. continuously contacting a mixture of ethylene diamine and monoethanolamine in a molar ratio of about 1 to 5 moles of ethylenediamine per mole of monoethanolamine with said pelleted catalyst at a temperature of about 250.degree. to about 400.degree. C. and a pressure of about 500 to about 3000 psig. to obtain an essentially noncyclic reaction product.
- 2. A method as in claim 1, wherein at least a portion of the diethylenetriamine reaction product is recycled to the reaction zone.
- 3. In a method wherein monoethanolamine is reacted with ethylenediamine in the presence of a phosphorous containing catalyst to provide an essentially noncyclic product comprising polyethylenepolyamines, the improvement for conducting said process on a continuous basis which comprises:
- a. using, as the catalyst, a catalyst composition consisting essentially of thermally activated calcined pellets of titania having thermally chemically bonded to at least the surface thereof about 0.5 to about 10 wt. % of phosphorous, said catalyst having been prepared by impregnating titania pellets with polyphosphoric acid, heating said impregnated pellets at a temperature of about 100.degree. to about 150.degree. C. for a period of time ranging from about 0.5 to 5 hours, and thereafter water washing, recovering and drying the thus-treated pellets,
- b. continuously contacting a mixture of ethylenediamine and monoethanolamine in a molar ratio of about 2 to 5 moles of ethylenediamine per mole of monoethanolamine with said pelleted catalyst at a temperature of about 250.degree. to about 400.degree. C. and a pressure of about 500 to about 3000 psig to obtain an essentially noncyclic reaction product comprising diethylenetriamine.
- 4. A method as in claim 3, wherein at least a portion of the diethylenetriamine reaction product is recycled to the reaction zone.
- 5. In a method wherein monoethanolamine is reacted with ethylenediamine in the presence of a phosphorous containing catalyst to provide an essentially noncyclic product comprising polyethylenepolyamines, the improvement for conducting said process on a continuous basis which comprises:
- a. using a catalyst prepared by a process consisting essentially of the steps of impregnating pellets of titania with polyphosphoric acid, heating said impregnated pellets at a temperature of about 100.degree. to about 150.degree. C. for a period of time ranging from about 0.5 to about 5 hours to thermally chemically bond from about 0.5 to about 10 wt. % of phosphorous to at least the surface of said pellets, and thereafter water washing, recovering and drying the thus-treated pellets,
- b. continuously contacting a mixture of ethylenediamine and monoethanolamine in a molar ratio of about 2 to 5 moles of ethylenediamine per mole of monoethanolamine with said pelleted catalyst at a temperature of about 300.degree. to about 350.degree. C. and a pressure of about 1000 to about 2000 psig to obtain an essentially noncyclic reaction product comprising diethylenetriamine.
- 6. A method as in claim 5, wherein the dried pellets are calcined at a temperature of about 200.degree. to about 800.degree. C. for a period of time within the range of about 2 to 24 hours.
Parent Case Info
This is a division of application Ser. No. 06/455,159, filed Jan. 3, 1983.
US Referenced Citations (10)
Foreign Referenced Citations (1)
Number |
Date |
Country |
2092467 |
Jan 1982 |
GBX |
Non-Patent Literature Citations (2)
Entry |
A. Winkler & E. Thilo (Deutsche Akad. Wiss. Berlin, Germany) Z. Anurg Chem 346 (1-2) 65 C.A. 14807c, 1966. |
Brennan U.S. application Ser. No. 453,841 filed 12/27/82, "Preparation of Linear Polyethylenepolyamines with Aluminum Phosphate Catalyst". |
Divisions (1)
|
Number |
Date |
Country |
Parent |
455159 |
Jan 1983 |
|