Method of producing aqueous solution of n-methylmorpholine-n-oxide

专利摘要:
The invention relates to the production of heterocyclic substances, in particular the preparation of an aqueous solution of N-methylmorpholine-M-oxide - a solvent for cellulose. The purpose of the invention is to simplify the process. The latter is carried out by mixing N-methylmorpholine with water in a mass ratio
公开号:SU1456011A3
申请号:SU874202567
申请日:1987-05-21
公开日:1989-01-30
发明作者:Шолтен Гейнц；Риндторфф Клаус
申请人:Хюльс Аг (Фирма)；
IPC主号:

专利说明:

one
The invention relates to the production of n-1-amine oxide, in particular an improved process for the preparation of an aqueous solution of N-methylmorpholine-N-hydroxide, which is used 5 as a solvent for cellulose.
The purpose of the invention is to simplify the process by mixing N-methylmorpholine and water in a weight ratio of 10 (50-75) :( 25-50), azeotropic distillation of this mixture, and the interaction of the azeotrope thus obtained, containing 74.5-75.1 % N-metipmorpholine with a 30-65% aqueous solution of hydrogen peroxide at 60-100 ° C and a molar ratio of N-methylmorpholine: hydrogen peroxide 1: (O, 75-0.9), followed by concentration of the reaction solution to the content
15
20
five
ten
15
20
N-methylmorpholin-N-oxide, equal to 59.4-60.1%, by distillation of water.
Example 1. 600 g of N-methylmorpholine and 600 g of water (50:50 weight ratio) are subjected to distillation with a reflux number 1 in a packed column 2 m high. 705 g of azeotrope are taken from the head portion. The product contains 74.5% N-methylmorpholine. 680 g of N-methylmorpholine azeotrope and water, while stirring, are reacted with 400 g of 35% aqueous hydrogen peroxide at 70 ° C for 2 hours, and then continue to stir for 6 hours at 68 ° C. At that, the molar ratio of N-methylmorpholine and hydrogen peroxide is 1: 0.82.
In vacuum, concentrate to 803 g. An aqueous solution of N-methylmor is obtained.
but
 cm
3, U
Follin-N-oxide of the following composition: N-Methylmorpholyn-N-oxide,% 59.4
Peroxide (calculated as Hj02), h, / ml2
Y-1miletilmorpholine,% 0.1
Acid number, mgKOH / g0.1
The water removed by distillation contains 34 May. 7, N-methylmorpholine. After concentration by distillation, it is reused.
Example 2. 600 g of N-methylmorpholine and 400 g of water (weight ratio .60: 40) are distilled with a reflux number 1 in a packed column 2 m in height. 700 g of azeotrope are taken from the head portion. Prodzpst contains 74.8% N-methylmorpholine,
680 g of N-methylmorpholine azeotrope and water, when stirred, are reacted with 197 g of 65% aqueous hydrogen peroxide at 60 ° C in
for 3 hours and then continue to stir for 6 hours at 60 ° C. The molar ratio of N-methylmorpholine and hydrogen peroxide is 1: 0.75. In vacuum, concentrate to 803 g. An aqueous solution is obtained.
N-methylmorpholyn-N-oxide of the following composition:, N-Methylmorpholine-Noxide,% 60.1
Peroxide (calculated
as H j), h / ml3
N-methylmorpholine,% 0.1
Acid number, mgKOH / g 0.1
The water removed by distillation contains 34% by weight of N-methymphorpholine.
After concentration by distillation, it is reused.
Example 3. 600 g of N-methylmorpholine and 200 g of water (weight ratio 75:25) are subjected to distillation with reflux number 1 in a packed column 2 m high. 685 g of azeotrope are taken from the head portion. Prop product contains 75.1% N-methylmorpholine
50
WITH

five
0
five
0
one
675 g of azeotrope N-metschIMopfolina and water with stirring is subjected to interaction with 512 g of 30% aqueous hydrogen peroxide for 90 minutes, and then continue to stir for 4 hours at 98 ° C. In this case, the molar ratio of N-methylmorpholine and hydrogen peroxide is 1: 0.9. In vacuum, concentrate to 803 g. An aqueous solution of N-methylmorpholyn-N-oxide is obtained of the following composition:
N-Methylmophorin-Nokyid,% 59.5
Peroxide (calculated
as), h. / MP1
N-methylmorpholine,% 0.1
Acid number, mgKOH / g0.1
The water removed by distillation contains 34% by weight of N-methylmorpholine. After concentration by distillation, it is reused.
The proposed method allows to simplify the process by reducing the number of stages from 7 to 3.

权利要求:
Claims (1)
[1]
Invention Formula
A method for producing an aqueous solution of N-methylmorpholyn-N-hydroxide by mixing N-methylmorpholine with water and reacting with an aqueous solution of hydrogen peroxide when heated, is characterized in that, in order to simplify the process, a mixture of N-methyl morpholine and water in mass ratio (50-75) :( 25-50) is subjected to azeotropic distillation and the resulting azeotrope containing 74.5-75.1% of N-metstmorpholine is supplied to react with a 30-65% aqueous solution of hydrogen peroxide at a temperature of 60-100 ° C and a molar ratio of N-methylmorpholine and hydrogen peroxide, equal to Volume 1: (O, 75-0,9), followed by concentrating the reaction solution to a N-content metilmopfolin-N-okcida equal 59,4-60,1% by distillation of water.

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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DE19863618352|DE3618352A1|1986-05-31|1986-05-31|METHOD FOR PRODUCING AQUEOUS N-METHYLMORPHOLIN-N-OXIDE SOLUTIONS|

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