Process for the preparation of isocyanates in the gas phase
US-9024057-B2 · May 5, 2015 · US
US9376377B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9376377-B2 |
| Application number | US-201414905026-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jul 21, 2014 |
| Priority date | Jul 26, 2013 |
| Publication date | Jun 28, 2016 |
| Grant date | Jun 28, 2016 |
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The invention relates to a method for producing an isocyanate by reacting the corresponding primary amine with phosgene in a reactor ( 100 ) which comprises at least one reaction zone ( 110 ) and a quenching zone ( 120 ) arranged below said reaction zone, having the following steps: (i) introducing a gaseous amine flow ( 1 ) and a gaseous phosgene flow ( 2 ) into the reactor ( 100 ) and reacting the flows in the reaction zone ( 110 ) into a product gas flow ( 3 ) comprising isocyanate and hydrogen chloride and optionally excess phosegene; (ii) introducing the product gas flow ( 3 ) into the quenching zone ( 120 ), in which the product gas flow is cooled by injecting a quenching liquid ( 4 ) via at least one quenching nozzle ( 200 ) such that a liquid flow ( 5 ) comprising the quenching liquid ( 4 ) and isocyanate and a gaseous flow ( 6 ) comprising hydrogen chloride and optionally phosgene are obtained; and (iii) separating the isocyanate from the liquid flow ( 5 ) obtained in step (ii); wherein the temperature T w *, of the wall of the reaction zone ( 110 ) directly above the quenching zone ( 120 ) is kept at a value which lies maximally 4.0%, preferably maximally 2.0%, below the maximum temperature, T w max , of the wall of the reaction zone, said maximum temperature being specified in Kelvin.
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The invention claimed is: 1. A method for producing an isocyanate by reacting the corresponding primary amine with phosgene in a reactor which comprises at least one reaction zone and a quenching zone arranged below the reaction zone, comprising: (i) introducing a gaseous amine stream and a gaseous phosgene stream into the reactor and reacting the mixture in the reaction zone to form a product gas stream comprising isocyanate and hydrogen chloride; (ii) introducing the product gas stream into the quenching zone in which the product gas stream is cooled by spraying in a quench liquid via at least one quench nozzle in such a manner that a liquid stream comprising quench liquid and isocyanate is obtained; and (iii) isolating the isocyanate from the liquid stream obtained in step (ii); wherein the temperature of the wall of the reaction zone immediately above the quenching zone is maintained at a value which is at most 15% below the maximum temperature in Kelvin of the wall of the reaction zone. 2. The method of claim 1 , in which the temperature of the wall of the reaction zone immediately above the quenching zone is held at a value which is at most 2.0% below the maximum temperature in Kelvin. 3. The method of claim 1 , in which the requirement of the temperature of the wall of the reaction zone immediately above the quenching zone is achieved by at least one of the following measures: (a) insulation of the reactor wall externally, (b) heating the reactor wall from the outside, and (c) insulation between wall of the reaction zone and wall of the quenching zone. 4. The method of claim 1 , in which the requirement of the temperature of the wall of the reaction zone immediately above the quenching zone is achieved by at least one of the following measures: (a) increasing the temperature of the quench liquid, and (b) decreasing the amount of quench liquid sprayed in. 5. The method of claim 1 , in which, when a single quench nozzle is used, the quench nozzle, or, when a plurality of quench nozzles are arranged successively in the direction of flow of the product gas stream, at least the first quench nozzles in the direction of flow of the product gas stream is/are oriented in such a manner that the linear elongation of the nozzle tube/the nozzle tubes is/are at an angle to the direction of flow of the product gas stream of 20° to 80°. 6. The method of claim 1 , in which, when a single quench nozzle is used, the quench nozzle, or, when a plurality of quench nozzles are arranged successively in the direction of flow of the product gas stream, at least the first quench nozzles in the direction of flow of the product gas stream is/are orientated in such a manner that the linear elongation of the nozzle tube/the nozzle tubes is/are at an angle to the direction of flow of the product gas stream of 50° to 80°. 7. The method of claim 1 , in which, when a single quench nozzle is used, the quench nozzle, or, when a plurality of quench nozzles are arranged successively in the direction of flow of the product gas stream, at least the first quench nozzles in the direction of flow of the product gas stream, is/are orientated in such a manner that the linear elongation of the nozzle tube crosses the wall of the quenching zone at a point which is beneath the start of the quenching zone by at least the distance L, wherein L=15 cm. 8. The method of claim 1 , in which, when a single quench nozzle is used, the quench nozzle, or, when a plurality of quench nozzles are arranged successively in the direction of flow of the product gas stream, at least the first quench nozzles in the direction of flow of the product gas stream, is/are orientated in such a manner that the linear elongation of the nozzle tube crosses the wall of the quenching zone at a point which is beneath the start of the quenching zone by at least the distance L, wherein L=70 cm. 9. The method claim 1 , in which the primary amine is selected from the group consisting of the isomers of toluylenediamine, the isomers of methylenediphenyldiamine, the isomers of naphthyldiamine, 1,6-hexamethylenediamine, the isomers of isophorenediamine, and the isomers of diaminodicyclohexylmethane.
by reaction of amines with carbonyl halides, e.g. with phosgene · CPC title
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