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: 2007-10-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Application Information

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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 polycondensa

Method used

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

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Experimental program
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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

[0060] 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

[0062] 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 continually preparing valeraldehyde, which reacts 1-butene raw material continually containing a little of trans/cis-2-butene, isobutene, butane with synthesis gas in the presence of the organic phosphinerhodium catalyst and triphenylphosphine. The process of the invention includes a reaction region, separation region and an activation region. Butene hydroformylation reaction liquid is evaporated, condensed and separated to two streams of raw product and circulating catalyst solution by film evaporation equipment, under shielding gas atmosphere of synthesis gas, and activated circulating catalyst solution enters reactor again. The present invention activates rhodium catalyst by catalyst activator, and controls or reduces acetal high boiling point byproducts which are generated by aldehyde polycondensation, enhance catalyst activity and regioselectivity of aldehyde. The film evaporation equipment used in the present invention is more effective than flash evaporator to separate catalyst solution and valeraldehyde producers in reaction liquor. Appropriate operational condition of film evaporation equipment can reduce or not generate aldehyde condensation, protive rhodium catalyst, enhance catalyst activity and prolong usage time of 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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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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