Professional Documents
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(54)
2,823,236 A
MONOETHANOLAMINE,
DIETHANOLAMINE AND
3,585,239 A
4,355,181 A
TRIETHANOLAMINE
4,847,418 A
6,075,168 A
*
*
LudWigshafen (DE)
Notice:
Sep. 5, 2001
(51)
(52)
(58)
CONTINUOUS PREPARATION OF
(30)
US 6,696,610 B2
(*)
(56)
References Cited
7/1989
6/2000
OTHER PUBLICATIONS
(57)
ABSTRACT
4/1933
U.S. Patent
Sheet 1 0f 4
US 6,696,610 B2
FIG.1
90,00
85,00
80,00
75,00
//
70,00
65,00
03 50,00
255,00
0 50,00
45,00
40,00
35,00
1
/
30,00
0
0,5
1,5
Q/m[MW / t (MEA+DEA+TEA)]
2,5
U.S. Patent
F|G.3
Sheet 3 0f 4
US 6,696,610 B2
U.S. Patent
Sheet 4 0f 4
US 6,696,610 B2
190
180
F|G.4A 170
160
150
140
130
120
110
100
F|G.4B
70
mol%
F|G.4C
2 -0EO
[vkmoI/h]
US 6,696,610 B2
1
CONTINUOUS PREPARATION OF
MONOETHANOLAMINE,
DIETHANOLAMINE AND
TRIETHANOLAMINE
10
25
35
45
55
reaction Zone compared With the reactor feed and thus an 65 ammonia to ethylene oxide With the feed to the reactive
US 6,696,610 B2
3
depleted of ammonia.
10
completely reacted.
ration column for ammonia and Water on the one hand and
MEA, DEA and TEA on the other hand, the ammonia- and
35
be separated into ammonia and Water on the one hand and 45 position betWeen the 1st and 15th theoretical plate, particu
into the ethanolamines on the other hand in a single distil
larly preferably from the 1st theoretical plate, to pass it into
lation column at atmospheric pressure, With condenser at the
one or more residence-time vessels, for example one or more
tubular reactors and, after a reaction has taken place, to
head of the column, using river Water as cooling medium. It
55
Speci?cally:
65
US 6,696,610 B2
5
EXAMPLE 1
10
procedure, taking as a basis a feed stream 2 of 5321 kg/h of
FIG. 4c as a function of the reaction rates (v) in kmol per
ethylene oXide, 2776 kg/h of ammonia, corresponding to an
hour (kmol/h), in each case based on the theoretical plates
ammonia/ethylene oXide molar ratio of 1.311 and 4000 kg/h
nth.
of Water, With an energy input of 2500 kiloWatts via the
The theoretical plates are in this case counted from head
evaporator at the bottom and of 3250 kiloWatt via an
to bottom in the reaction distillation column I.
15
intermediate evaporator at the 31st plate gave a bottom
The curve in FIG. 1 shoWs that the MEA concentration in
TEA)].
20
25
Stream No.
35
H2O
NH3
EO
MEA
DEA
40 TEA
Total amount
100.0
33.2
9.8
0.2
34.5
16.9
5.6
12083
60.4
29.6
9.8
6904
100.0
77.1
22.9
100.0
10
5321
1573
500 ppm
5179
kg/h
EXAMPLE 2
45
With the same plant and the same process parameters, but
With a loWer input of energy of only 3450 kW, streams 1 to
6, Which have the same meaning as in eXample 1, Were
Proportion by
Weight
[070]
TABLE 1
30
50
Stream-No.
55
Proportion by
Weight
[070]
H2O
NH3
EO
MEA
60 DEA
TEA
Total amount
100.0
100.0
33.2
9.8
0.2
28.5
18.9
9.6
12083
49.9
33.1
16.8
6904
77.2
22.8
100.0
10
5430
1464
500 ppm
5179
kg/h
65
US 6,696,610 B2
8
7
Weight of the ethanolamines MEA+DEA+TEA (CMEA [%])
We claim:
1. A continuous process for the preparation of
25
ethanolamine.
7. A process as claimed in claim 1, Wherein the reactive
distillation column is operated at a column pressure of from
10 to 80 bar absolute.
8. A process as claimed in claim 1, Wherein, from the
distillation column, to separate ammonia and Water on the
one hand monoethanolamine, diethanolamine and triethano
lamine on the other hand, the ammonia- and Water
containing head product is returned via a condenser on the
head of the reactive distillation column, to the head region
thereof.
9. A process as claimed in claim 1, Wherein some of the
input of energy to the evaporator at the bottom is replaced
45