Arrangement for manufacturing ethylene glycol and ethanolamines

专利摘要:
The invention relates to a ruthenium promoted nickel and/or cobalt dehydrogenation-hydrogenation catalyst. The ruthenium on the catalyst is applied from a solution containing a ruthenium halide compound. The catalyst use in organic reactions and a process performed in its presence are also described. Preferably, the catalyst is used to aminate alkylene oxides, alcohols, phenols, alkanolamines, aldehydes, and ketones.
公开号:SU1440331A3
申请号:SU3792256
申请日:1984-09-07
公开日:1988-11-23
发明作者:Келль Йюхан
申请人:Берол Кеми Аб (Фирма)；
IPC主号:

专利说明:

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about
00
00
The invention relates to catalysts for dehydrogenation - hydrogenation, in particular for the aminating of ethylene glycol and ethanolamines.
The purpose of the invention is to increase the selectivity of the catalyst for primary and non-cyclic amines due to the additional content of ruthenium at a certain ratio of components and a certain structure,
Example 1. A K90g catalyst carrier — activated alumina, taken in the form of tablets with a length and diameter of about 3 mm and a surface area of about 100, is added to a concentrated aqueous solution of metal nitrates, the nature and quantities of which are indicated in Table. 1. The excess liquid is evaporated under vacuum, the tablets are dried, and the nitrates are decomposed to the corresponding oxides by exposure to a stream of dry air at 500 ° C. After cooling, the tablets are impregnated with a 2% aqueous solution of ruthenium compound and dried at 100 ° C in air.
The tablets are then heated in a stream of hydrogen, first for 1 hour at 150–200 s in order to convert the ruthenium
Research institute
for reducing the metal oxides to the metallic state in finely divided form.
In all catalysts table. 1, the content of activated alumina is 99.0% by weight, based on the weight of the carrier, with the exception of catalysts A3 and OZ, where it is 99.8%.
Example 2. In a 300 ml autoclave equipped with a stirrer and automatic temperature control, purge with nitrogen. 8 g of one of the catalysts prepared in accordance with Example 1, 25 g of monoethanolamine, 3.5 water and 65 g of liquid ammonia are loaded into the autoclave. The autoclave is closed and hydrogen is supplied under a pressure of 5.5 MPa. The content of the auto clava is heated to and maintains the set temperature with continuous stirring until the completion of the experiment.
In the course of the reaction, samples are taken from the autoclave and analyzed by gas-liquid chromatography. Disconnection in the metal root and then for 4 hours at 400 ° C
0
five
0
five
0
Q
five
five
0
five
The conversion of the aminated compound is read and the amounts of products obtained in the reaction are determined. The results are presented in table. 2
Conversion is defined as the ratio of the amount of the starting compound abused in the reaction to the initial amount.
Example 3. A mixture of 6.25 g of diaethanolamine and 18.75 g of monoethanolamine with ammonia is reacted in accordance with Example 2. The catalyst A1 described in Example 1 is used in the reaction. Catalyst B1 is used for comparison.
Example 4. A mixture of 6.25 g of amino-ethylethanolamine and 18.75 g of monoethanolamine with ammonia is carried out in accordance with Example 3,
Example 5. Analogously to Example 3, a mixture of 12.5 g of monoethylene glycol and 12.5 g of monoethanolamine with ammonia was reacted. Obtained in examples 2-3 data are given in table. 3
From the data in Tables 2 and 3, it follows that the proposed catalysts have an advantage with respect to the formation of primary amino groups.
Examples 6-20. Four catalyst catalysts are prepared according to the procedure of Example 1, but using different amounts of metal compounds and on various supports. The catalysts have the composition specified in table. four.
The catalysts are then tested in the same manner as in example 2, while obtaining the results presented in table. five.
Thus, the proposed catalyst has a high selectivity for primary and non-cyclic amines.

权利要求:
Claims (2)
[1]
1. The catalyst for the amination of ethylene glycol and ethanolamines, including nickel and / or cobalt and a carrier containing alumina and / or silica, characterized in that, in order to increase the selectivity of the catalyst for primary and non-cyclic amines, it also contains ruthenium the following content of components, wt.%:
Nickel and / or
cobalt 4.0-40.0 Ruthenium 0.1-5.0 Carrier 55.0-95.9 and has a structure obtained by impregnating a carrier containing nickel and / or cobalt in the form of metals or oxides with a solution of halogen-containing
ruthenium compounds, followed by drying and reduction in a stream of hydrogen at elevated temperature to metallic ruthenium.
[2]
2. A catalyst according to claim 1, characterized in that the carrier contains 95-100% by weight of activated alumina.
 Table 1
Ruthenium
Ruthenium hydrochloride 0.50
Ruthenium halohydrate 0.50
Also
99.55 90.00 89.55
89.55 90.00 88.03
0.49
87,81
0.97
87.39
Continued table. one
L p
yech "pia. EDA - etkpend am n; KEA - mokoetaiopamni; AEP - “Minoathyl pvraai; 1P shteraei) DETA - diethylenes; AEBA - oampshit olamp; B2iP - oxyepiti erae k; DEL - d this olamine,
Ie-ea difficulties analyzing this component t ve defined.
AI2 Nickel 10 5 Alumina (99 wt.% 85
activated A1 „0)
A13 Cobalt 40 0.5, 5
A14 Nickel 4 0.1 Alumina (95% by weight of activated alumina) 95.9
A15 10 0.5 Activated alumina 89.5
(98 wt.% Activated alumina)
Continued gab.2
Table n 3
Table 4
Table

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同族专利:

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公开号 | 公开日

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US4855505A|1989-08-08|

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MX167905B|1993-04-21|

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NO160118B|1988-12-05|

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IN162724B|1988-07-02|

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SE461095B|1990-01-08|

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US4701434A|1987-10-20|

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AT51394T|1990-04-15|

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KR910008723B1|1991-10-19|

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BR8404488A|1985-07-30|

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EP0146508A3|1985-08-14|

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NO843575L|1985-03-11|

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DD228181A5|1985-10-09|

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IE842255L|1985-03-09|

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AU565044B2|1987-09-03|

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NO160118C|1989-03-15|

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DE3481768D1|1990-05-03|

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CA1225079A|1987-08-04|

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EP0146508A2|1985-06-26|

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DK161944B|1991-09-02|

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FI81027B|1990-05-31|

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FI843514L|1985-03-10|

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ZA846989B|1985-04-24|

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IE57631B1|1993-02-10|

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ES8601724A1|1985-11-01|

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FI843514A0|1984-09-07|

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SE8304828L|1985-03-13|

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DK428484D0|1984-09-07|

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DK161944C|1992-02-03|

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SE8304828D0|1983-09-09|

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ES535750A0|1985-11-01|

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FI81027C|1990-09-10|

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UA5761A1|1994-12-29|

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JPH0518627B2|1993-03-12|

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EP0146508B1|1990-03-28|

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AU3378384A|1985-03-14|

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DK428484A|1985-03-10|

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JPS6084143A|1985-05-13|

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KR850002042A|1985-05-06|

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GR80295B|1984-12-18|

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法律状态:
2005-10-20| REG| Reference to a code of a succession state|Ref country code: RU Ref legal event code: MM4A Effective date: 20030908 |

优先权:

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申请号 | 申请日 | 专利标题

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SE8304828A|SE461095B|1983-09-09|1983-09-09|AMINING PROCEDURE USING A RUTENIUM DOPPED NICKEL AND / OR COVOLT CATALYST|LV930068A| LV5195A3|1983-09-09|1993-01-26|Catalyst for ethylene glycol and ethanolamine amines|

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LTRP483A| LT2073B|1983-09-09|1993-04-09|CATALYST ETHYLENGLICOL AND ETHANPLAMIN FOR MIXING|