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Preparation process of 2-ethyl hexenal and 2-ethyl hexanol

A preparation technology of ethylhexenal and 2-ethylhexenal, which is applied in the field of preparation technology of 2-ethylhexenal and 2-ethylhexanol, can solve the problems of complex process, high energy consumption, side reactions, etc., and achieve simplification Process, increase the concentration of alkali, the effect of mild reaction process

Active Publication Date: 2014-02-19
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, in the three reaction loops of the n-butyraldehyde condensation part, the first loop is passed into fresh alkaline catalyst aqueous solution, and in the first loop, the condensation reaction intensity is larger, the reaction is faster, and it is easier to generate polybutyraldehyde, polybutyraldehyde, Byproducts such as 2-ethyl-4-methylpentenal; secondly, the alkali concentration of the fresh alkaline catalyst aqueous solution is usually controlled as 2%, if the concentration of the fresh alkali solution is increased, side reactions are more likely to occur, and the condensation reaction itself will have Water is generated, therefore, there will be a large amount of dilute alkaline wastewater produced; again, the n-butyraldehyde content in the butyraldehyde raw material suitable for condensation requires ≥99.8%, so a rectification tower with more than 100 plates is required to remove the isobutyraldehyde Butyraldehyde impurity removal, high energy consumption, and complex process

Method used

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  • Preparation process of 2-ethyl hexenal and 2-ethyl hexanol
  • Preparation process of 2-ethyl hexenal and 2-ethyl hexanol
  • Preparation process of 2-ethyl hexenal and 2-ethyl hexanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] like image 3 As shown, a system for preparing 2-ethylhexenal provided by the present invention includes a first reactor 311, a second reactor 312, a first chromatograph 331 and a second chromatograph 332; wherein , the outlet of the first reactor 311 is connected to the inlet of the first chromatograph 331 through a heat exchanger 361 through a pipeline; the lower layer outlet of the first chromatograph 331 communicates with the outside world through the lye circulation pump 321, and the first chromatograph The upper floor outlet of 331 is connected with the inlet of the second reactor 312 through a pipeline; the lye inlet of the second reactor 312 is connected with the lye tank 38 through the lye supply pump 35, and the outlet of the second reactor 312 is connected with the second The inlet of chromatograph 332 is connected through pipeline through heat exchanger 362; The outlet of the upper layer is connected to the downstream process through the pipeline through th...

Embodiment 2

[0046] The process flow is attached image 3 , Fresh raw material 100ml / min containing 99.8wt% n-butyraldehyde enters the first condensation reactor 311 with the alkaline catalyst aqueous solution 31.2ml / min from the lye circulating pump 322, mixes and reacts, and the reaction temperature is 80°C. The residence time is 15 minutes. After the discharge from the first condensation reactor 311 is cooled to 40°C by the cooler 361, it is sent to the chromatograph 331 for stratification. Reprocessing, upper layer butyraldehyde and octenal mixed solution (56.4wt% of 2-ethylhexenal content), is sent in the second condensation reactor 312 with 85ml / min, with the 47ml from lye supply pump 5 After the 2wt% lye of / min is mixed, react further, reaction temperature 120 ℃, residence time 10min, the output of the second condensation reactor 312 is sent into chromatograph 332 after cooler 362 is cooled to 40 ℃, through layer Impurities such as 2-ethylhexenal 97wt% and polybutyraldehyde 0.7%, ...

Embodiment 3

[0048] The process flow and reaction conditions are the same as in Example 2, except that the raw materials are fresh 99wt% n-butyraldehyde and 1wt% isobutyraldehyde. After the first condensation reactor 311 completes the reaction, the chromatograph 331 is layered, and the upper layer butyraldehyde and octenal mixed solution (the content of 2-ethylhexenal is 53.1wt%) is reacted 322 through the second condensation reactor. , separated by chromatography 332 to obtain the upper layer solution is 96.4wt% of 2-ethylhexenal and 0.7% of polybutyraldehyde, 0.17% of 2-ethyl-4-methylpentenal and unreacted n-butyraldehyde 1% and other impurities. After hydrogenation and rectification, the final product of 2-ethylhexanol with a purity of ≥99.6% is obtained. The main impurities of the product are 0.14% of 2-ethyl-4-methylpentanol, 0.12% of water, and 2-ethylhexanol Aldehyde 0.05%.

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Abstract

The invention provides a preparation process of 2-ethyl-hexenal and 2-ethyl hexanol. The preparation process comprises the following steps: carrying out condensation reaction and dehydration reaction on butyraldehyde used as a raw material under the catalysis action of an alkaline catalyst in a first reactor and a second reactor which are connected in series, thus generating 2-ethyl hexenal, wherein the raw material butyraldehyde contacts the alkaline catalyst aqueous solution in the reactors in a counter-flow mode, and the fresh alkaline catalyst aqueous solution is added into the second reactor. In the process provided by the invention, the reaction occurring in the reactors is milder and has less possibility to generate by-products, therefore the raw material butyraldehyde for the condensation reaction can be directly introduced into an aldehyde condensation section for the condensation reaction as long as the content of n-butyraldehyde in the raw material butyraldehyde is not less than 90wt%; and furthermore, the alkali concentration of the fresh alkaline catalyst is improved, and the emission of the alkaline wastewater is reduced. In addition, crude 2-ethyl hexenal products containing a small amount of impurities, prepared by the preparation process, can be introduced into hydrogenation and rectification sections to prepare 2-ethyl hexanol products.

Description

technical field [0001] The invention relates to a preparation process of 2-ethylhexenal and 2-ethylhexanol, which belongs to the technical field of chemical industry. Background technique [0002] 2-Ethylhexanol (commonly known as octanol) is a colorless oily liquid with luster and fruity aroma. It has the largest output in oxo synthesis, accounting for more than half of the total oxo alcohol. 2-Ethylhexanol is mainly used in the production of the plasticizer dioctyl phthalate in the plastic industry and as a plasticizer for polyvinyl chloride resin. It has a good compatibility with most synthetic resins and rubbers used in industry. Solvent effect, high plasticizing efficiency, low volatility, good low temperature softness, good heat resistance and corrosion resistance. 2-Ethylhexanol is also used as a raw material for synthetic lubricants and antioxidants. It is also a solvent and a defoamer with good performance. It can be used in paper pulp sizing, photography, paint, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/21C07C45/72C07C31/125C07C29/141C07C29/17
Inventor 张佶璘蒋文陈建伟
Owner SHANGHAI HUAYI ENERGY CHEM
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