Method for isomerizing cis-piperylene
A technology of cis-piperene and isomerization, which is applied in the direction of isomerization to hydrocarbon production, organic chemistry, etc., can solve the problems of loss of catalytic activity, unstable complexes, etc., to improve stability and improve stability. , improve the effect of selectivity
Active Publication Date: 2014-12-17
SHANGHAI PEARLK CHEM
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Problems solved by technology
But as in "Die Aktivierung von molekularem Wasserstoff durch homogene Katalyse in flüssiger Phase, 2.Die Kinetik der Aktivierung in lendiamincobalate (Ⅱ)- "["Zeitschrift für physikalische Chemie,1966,49"] the research carried out shows that due to [Co(CN) 3 EN] -1 The inherent instability of the complex itself, [Co(CN) 3 EN] -1 The divalent cobalt ions of the complex are easily oxidized and converted into trivalent cobalt ions, thus losing catalytic activity
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[0022] 1. Preparation of catalyst
[0023] The catalyst was prepared in a pressure-resistant, jacketed glass reactor with a volume of 1000 ml. The upper part of the glass reactor is equipped with a variable speed mechanical stirring device, a thermocouple for temperature measurement, a pressure gauge, hydrogen and nitrogen gas inlets and feeding ports. The reaction temperature is controlled by a constant temperature oil bath temperature. Accurately measured deionized water, Co(AC) 2 4H 2 O is added to the reactor through the feeding port, and the stirring is started and stabilized at 200 rpm, so that the Co(AC) 2 4H 2 O is dissolved in water to prepare a transparent aqueous solution; replace the reactor with nitrogen, and add potassium cyanide aqueous solution and EN (ethylenediamine) under the protection of nitrogen, and the prepared reaction solution is used as a catalyst, wherein [Co(CN) x EN]-(X-2) Co in the complex 2+ : CN - : See Table 1 for the molar ratio of EN ...
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The invention provides a method for isomerizing cis-piperylene. The method comprises the following steps of: (1) preparation of a [Co(CN)xEN]<-(X-2)> complex: preparing weighed Co(AC)2.4H2O into an aqueous solution under the protection of nitrogen, and adding a weighed potassium cyanide aqueous solution and diethylamine at a room temperature under a stirring condition for full reaction, wherein prepared reaction liquid serves as a catalyst, the molar ratio of Co<2+>: CN<->: EN in [Co(CN)xEN]<-(X-2)> complex is 1:(3.90-4.10):3, and the concentration of cobalt ions is 0.10-2.5mol / L; and (2) isomerization reaction of piperylene: feeding mixture gas of nitrogen and hydrogen to a reactor with the piperylene raw material, wherein the reaction temperature is 0-40 DEG C, the system pressure is 0.10-3.0 bar, the stirring rate is 300-800r / m, the usage amount of the catalyst accounts for 1-10% of the mass of the piperylene by the mass of cobalt, and the reaction time is 10-300 minutes. The method has the advantages of obviously improving the isomerization performance of the catalyzed cis-piperylene, effectively promoting the selectivity of reaction and having essential characteristics of engineering.
Description
technical field [0001] The present invention relates to a kind of method of cis-piperylene isomerization, particularly relate to cis-piperylene in complex catalyst [Co(CN) x EN] -(X-2) And in the presence of mixed gas of nitrogen and hydrogen, the method of converting into trans piperylene through isomerization reaction. Background technique [0002] Piperylene is mainly used in the production of carbon five aliphatic petroleum resins and methyl tetrahydrophthalic anhydride and its rehydrogenation to produce methyl hexahydrophthalic anhydride and other epoxy resin curing agents. Usually the piperylene product is a mixture of cis piperylene and trans piperylene, the total mass content of piperylene is generally between 68% and 72%, of which the mass content of trans piperylene is 42-46%, the mass content of cis-piperylene is 25-27%, the mass ratio of trans-piperylene to cis-piperylene is 1.67-1.74, and the other main components are cyclopentene and cyclopentene Alkanes, th...
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IPC IPC(8): C07C11/20C07C5/22
Inventor 石康明
Owner SHANGHAI PEARLK CHEM