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Process of continuously preparing n-pentanal

A process, n-valeraldehyde technology, applied in the field of continuous preparation of n-valeraldehyde by butene hydroformylation reaction, can solve the problem of increasing high-boiling point high polymer, increasing polycondensation of olefin hydroformylated aldehyde products, reducing catalyst activity, etc. question

Active Publication Date: 2009-08-12
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that if the reaction liquid is kept at a higher temperature for a long time, it will increase the polycondensation of olefin hydroformylation aldehyde products, increase the high boiling point high polymer, and reduce the catalyst activity.

Method used

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  • Process of continuously preparing n-pentanal
  • Process of continuously preparing n-pentanal
  • Process of continuously preparing n-pentanal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] In the reaction process shown in the accompanying drawing, the volume of the reactor is 1 liter, equipped with a speed-regulating double-layer electromagnetic stirrer, and heated by an oil bath jacket. The catalyst activator is electrically heated.

[0057] Add 3.84 g triphenylphosphine rhodium acetylacetonate and 369.8 g triphenylphosphine catalyst solution uniformly dissolved in 3.5 liters of n-valeraldehyde into the flow reaction system. Purge with high-purity nitrogen to replace the system air. Introduce purified H 2 / CO ratio of 1.0 syngas until the oxygen content of the system is below 0.1ppm. Add 1-butene purity 95.2wt% and isobutene 0.5wt% olefin raw material to react. The operating conditions of reactor R1 are controlled at 80-90°C and 1.9-2.1MPa. The reaction liquid is separated into the liquid phase at 60°C and 0.4-0.8MPa in the gas-liquid reactor V3, and sent to the thin-film evaporator V5 by the pump P1, and the crude product valeraldehyde is separated a...

Embodiment 2

[0061] Butene hydroformylation operation experimental method identical with embodiment 1. Add 1-butene with 80.8wt% purity of 1-butene and 1.5wt% isobutene as olefin raw material, and continue the hydroformylation reaction for 1020 hours. The results are listed in Table 1.

Embodiment 3

[0063] Butene hydroformylation operation experimental method identical with embodiment 1. Butene raw material composition is 1-butene 55.4wt%, cis / trans-2-butene 22.6wt%, butane 19.5wt%, isobutene 2.5wt%, continuous hydroformylation reaction for 50 hours, the results are listed in Table 1 .

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Abstract

The invention discloses a process for continuously preparing n-valeraldehyde. The process is a continuous reaction of 1-butene raw material containing a small amount of cis / trans-2-butene, isobutene and butane with synthesis gas in the presence of organophosphine carbonyl rhodium catalyst and triphenylphosphine to prepare n-valeraldehyde . The technological process of the present invention includes a reaction zone, a separation zone and an activation zone. In the flow reaction device, the butene hydroformylation reaction liquid is evaporated and condensed under the protective atmosphere of synthesis gas by thin film evaporation equipment, and separated into two streams: the crude product and the circulating catalyst solution. The circulating catalyst is activated and then enters reactor. The invention adopts a catalyst activator, activates the rhodium catalyst, controls or reduces the acetal by-product with high boiling point generated in the aldehyde polycondensation reaction, improves the activity of the catalyst, and improves the regioselectivity of the aldehyde. The film evaporation equipment selected by the present invention is more effective than the flash evaporator in separating the catalyst solution and the valeraldehyde product in the reaction liquid. Appropriate operating conditions of the film evaporator can reduce or not produce aldehyde condensation, protect the rhodium catalyst, improve the catalyst activity and prolong the service life of the catalyst.

Description

technical field [0001] The invention relates to a process for preparing n-valeraldehyde by olefin hydroformylation. More precisely, the present invention relates to a process for the continuous preparation of n-valeraldehyde by hydroformylation of butene. Background technique [0002] The preparation of n-valeraldehyde by hydroformylation of butene is of great economic significance. N-valeraldehyde is an important intermediate in organic synthesis, widely used in spices, medicine, pesticides, coatings, mineral processing and other industries. 2-Propylheptanol produced by valeraldehyde condensation and hydrogenation reaction is an excellent PVC plasticizer raw material currently being developed and manufactured at home and abroad. [0003] For a long time, there have been many studies on the reaction process of butene hydroformylation to valeraldehyde in the world. The early industrial production of butene hydroformylation to prepare n-valeraldehyde used cobalt catalysts. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/49C07C47/02
Inventor 陈革新赵培庆张锦华赵志远夏春谷王金梅于超英陈谊凌文凯姚彩兰高国进
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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