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 containing titanium triphosphate and 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 phosphoric acid for a period of time ranging from about 0.5 to about 5 hours, thereafter water washing, recovering and drying the thus-treated pellets and then calcining the pellets at about 200.degree. C. to about 800.degree. C. for about 1 to about 24 hours,
- 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 the reaction product is fractionated to obtain at least a fraction comprising diethylenetriamine and wherein at least a portion of said diethylenetriamine is recycled to the reaction zone together with the said feedstock.
- 3. 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 a catalyst prepared by treating titania pellets with phosphoric acid for a period of time within the range of about 0.5 to about 5 hours sufficient to thermally chemically bond from about 0.5 to about 10 wt.% of phosphorus to at least the surface of said pellets and to convert at least a portion of the titanium and phosphorous to titanium triphosphate, and thereafter water washing, recovering and drying the thus treated pellets and then calcining said pellets at about 500.degree. to about 700.degree. C. for about 4 to about 16 hours,
- continuously contacting a mixture of ethylenediamine 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.
- 4. 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 the catalyst, a catalyst composition consisting essentially of thermally activated calcined pelleted titania containing titanium triphosphate and 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 impregnating titania pellets with phosphoric acid, heating the impregnated pellets at about 100.degree. to about 150.degree. C. for a period of time ranging from about 0.5 to about 5 hours, thereafter water washing, recovering and drying the thus-treated pellets and then calcining the pellets at about 200.degree. C. to about 800.degree. C. for about 1 to about 24 hours,
- 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.
- 5. A method as in claim 4, wherein the reaction product is fractionated to obtain at least a fraction comprising diethylenetriamine and wherein at least a portion of said diethylenetriamine is recycled to the reaction zone together with the said feedstock.
- 6. 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 a catalyst prepared by a process consisting of the steps of impregnating titania pellets with phosphoric acid, heating the impregnated pellets at a temperature of about 100.degree. to about 150.degree. C. for a period of time within the range of about 0.5 to about 5 hours sufficient to thermally chemically bond from about 0.5 to about 10 wt.% of phosphorus to at least the surface of said pellets and to convert at least a portion of the titanium and phosphorous to titanium triphosphate, and thereafter water washing, recovering and drying the thus treated pellets and then calcining said pellets at about 500.degree. to about 700.degree. C. for about 4 to about 16 hours,
- 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 300.degree. to about 350.degree. C. and a pressure of about 1000 to about 2000 psig. to obtain an essentially noncyclic reaction product.
Parent Case Info
This is a division of application Ser. No. 455,158, 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. Will. 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)
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Number |
Date |
Country |
Parent |
455158 |
Jan 1983 |
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