Method for producing KA oil through oxidizing cyclohexane by using air on basis of gas-liquid-solid heterogeneous reaction separation synchronization reactor

A multi-phase reaction and air oxidation technology, applied in the separation/purification of hydroxyl compounds, separation/purification of carbonyl compounds, chemical instruments and methods, etc., can solve the problem of increasing equipment investment and energy consumption, pollution of solvent environment, and reaction Reduce product selectivity and yield, increase the residence time of reaction products, etc., to achieve the effect of expanding the operable range, avoiding oxidation or decomposition, and solving the complex structure of equipment

CN103755521BActive Publication Date: 2015-02-18新疆普禾粟新型环保材料有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2015-02-18

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Abstract

The invention discloses a method for producing KA oil through oxidizing cyclohexane by using air on the basis of a gas-liquid-solid heterogeneous reaction separation synchronization reactor, wherein the water-containing cyclohexane is added into the reactor, the reactor comprises a reaction tower and at least two constant temperature settlement towers communicated with the bottom of the reaction tower, and the reaction tower is internally provided with a gas phase area, an oxidization area and a gas outlet; the oxidization area and the constant temperature settlement towers are filled with the cyclohexane in the reaction, the air is introduced continuously from the bottom of the oxidization area and is in contact with the cyclohexane to carry out the oxidization reaction, meanwhile, the produced KA oil is blended with water to form a KA oil phase, the KA oil phase is settled into the constant temperature settlement tower, the cyclohexane in the constant temperature settlement tower at the moment enters the oxidization area through an external circulation system, so that the reaction is conducted continuously, the KA oil phase continues to settle in the constant temperature settlement tower until the constant temperature settlement tower is fully filled the KA oil phase, then the reaction tower is switched to be communicated with the other constant temperature settlement tower filled with the cyclohexane, the operation is conducted on the constant temperature settlement towers alternatively to continuously produce the KA oil. The method is used to continuously produce the KA oil with high percent of conversion and high selectivity, the production efficiency is improved, and the production cost is lowered.
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Description

technical field

[0001] The invention relates to a process for producing KA oil by using air to oxidize cyclohexane, belonging to the field of KA oil production. Background technique

[0002] KA oil is a mixture of cyclohexanol and cyclohexanone, which is the basic chemical raw material for the production of Nylon 6 and Nylon 66. Industrially, liquid-phase air oxidation of cyclohexane is the main method for preparing KA oil. At present, the method for producing KA oil by oxidation of cyclohexane in industry is the non-catalyzed oxidation method of Stamica Company in the Netherlands. In this method, the liquid-phase air oxidation of cyclohexane is carried out under high temperature and high pressure conditions, and the reaction yield is low. Product selectivity is poor. At present, the best conversion rate of cyclohexane that can be achieved in industry is 4%, and the yield of KA oil is 82%. Patent CN1191218 discloses a method for preparing KA oil by air oxidation of cycloh...

Examples

Embodiment 1

[0040] use figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of cyclohexane and prepares KA oil product; Wherein, the diameter-to-height ratio of the bubbling gravity reaction tower is 1:20; The length of the gravity settling plate and the tower diameter ratio are 1: 0.8; the included angle of the gravity settling plate along the tower axis is 75°; there are two constant temperature settling towers, the constant temperature settling tower I and the constant temperature settling tower II; the outlet of the reaction liquid is 2 / 5 of the height of the tower body from the top of the reaction tower.

[0041] The cyclohexane raw material with a water content of 0.5wt% enters the constant temperature settling tower I and the bubbling gravity reaction tower from the upper reaction material inlet of the constant temperature settling tower I, and fills the oxidation zone of the constant temperature settling tower I and th...

Embodiment 2

[0045] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of cyclohexane to prepare KA oil product; wherein, the ratio of diameter to height of the bubbling gravity reaction tower is 1:40; the length of the gravity settling plate and the diameter ratio of the tower are 1: 1.2; The included angle of the gravity settling plate along the tower axis is 45°; there are two constant temperature settling towers, I and II; the outlet of the reaction liquid is 3 / 7 of the height of the tower body from the top of the reaction tower.

[0046] The cyclohexane raw material with a water content of 0.7wt% enters the constant temperature settling tower I and the bubbling gravity reaction tower from the upper reaction material inlet of the constant temperature settling tower I, and fills the oxidation zone of the constant temperature settling tower I and the bubbling gravity reaction tower, and circulates The tee on the p...

Embodiment 3

[0050] Attached figure 1 The shown gas-liquid-solid multiphase reaction separation synchronous reactor carries out the air oxidation of cyclohexane to prepare KA oil product; wherein, the ratio of diameter to height of the bubbling gravity reaction tower is 1:35; the length of the gravity settling plate and the diameter ratio of the tower are 1: 1.2; The included angle of the gravity settling plate along the tower axis is 55°; there are two constant-temperature settling towers, the constant-temperature settling tower I and the constant-temperature settling tower II; the outlet of the reaction liquid is 3 / 7 of the height of the tower body from the top of the reaction tower.

[0051] The cyclohexane raw material with a water content of 0.8wt% is added with cobalt naphthenate (concentration: 10ppm) as a catalyst, and the mixed solution enters the constant temperature settling tower I and the bubbling gravity reaction tower from the upper reaction material inlet of the constant tem...