Preparation method and preparation apparatus of high-grade 4-tert-butylbenzaldehyde

A technology of p-tert-butyltoluene and p-tert-butyl, applied in the chemical field, can solve the problems of limited gas-liquid contact area, tail gas emission pollution, low oxygen utilization rate, etc., achieve short reaction time, large gas-liquid contact area, The effect of high utilization

Pending Publication Date: 2017-07-25
NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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Problems solved by technology

However, this method has problems such as limited gas-liquid contact area, long reaction time, high reaction temperature, low oxygen utilization rate, and pollution caused by exhaust emissions.

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  • Preparation method and preparation apparatus of high-grade 4-tert-butylbenzaldehyde
  • Preparation method and preparation apparatus of high-grade 4-tert-butylbenzaldehyde
  • Preparation method and preparation apparatus of high-grade 4-tert-butylbenzaldehyde

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[0027] The invention provides a method for preparing high-grade p-tert-butylbenzaldehyde. The preparation method of high-grade p-tert-butylbenzaldehyde according to the embodiment of the present invention comprises the following steps:

[0028] A) Mix p-tert-butyltoluene, water and a halogen-free catalyst in a micro-bubble reactor and perform an oxidation reaction to obtain a reaction feed liquid;

[0029] B) oil-water separation is carried out to the reaction feed liquid, so as to obtain a water phase and an oil phase, the water phase contains a catalyst, and the oil phase contains p-tert-butylbenzaldehyde and impurities; and

[0030] C) Separating the p-tert-butylbenzaldehyde and the impurity to obtain high-grade p-tert-butylbenzaldehyde.

[0031] Since the high-grade p-tert-butylbenzaldehyde preparation method according to the embodiment of the present invention uses a halogen-free catalyst, the p-tert-butylbenzene prepared according to the high-grade p-tert-butylbenzaldeh...

Embodiment 1

[0071] The catalyst is dissolved in solvent water with a mass fraction of 1%, and p-tert-butyltoluene and solvent water are transported to the 100L microbubble reactor 5 by pump 3 and pump 1 according to the mass ratio of 1:1. When adding the feed liquid of 60 kg, that is, when the total weight of p-tert-butyltoluene, water and catalyst is 60 kg, stop feeding, open the pump 14, and make the flow rate of the feed liquid of circulation be 1000L / h, micron bubble reactor 5. The size of the generated bubbles is 500nm-500μm. The circulating feed liquid is heated through the heat exchanger 11. When the temperature rises to 50°C, oxygen is introduced into the micro-bubble reactor 5 to increase the pressure in the micro-bubble reactor 5. to 0.2MPa (gauge pressure).

[0072] After 1.6 hours of reaction, open the valve 15, pump 1 and pump 3, adjust the flow meter 16, and send the reaction material liquid to the phase separator 21 at a flow rate of 10L / h, so that the pump 1 and pump 3 rea...

Embodiment 2

[0076] The catalyst is dissolved in solvent water with a mass fraction of 1.2%, and p-tert-butyltoluene and solvent water are transported to the 100L microbubble reactor 5 by pump 3 and pump 1 according to the mass ratio of 1:1.5. When adding the feed liquid of 60kg, that is, when the total weight of p-tert-butyltoluene, water and catalyzer is 60 kg, stop feeding, open pump 14, make the flow of the feed liquid of circulation be 20000L / h, micron bubble reactor 5 The size of the generated bubbles is 50 μm-1000 μm, and the circulating feed liquid is heated through the heat exchanger 11. When the temperature rises to 90°C, oxygen is introduced into the micro-bubble reactor 5 to reduce the pressure in the micro-bubble reactor 5. Rise to 0.3MPa (gauge pressure).

[0077] After reacting for 0.1 hour, open the valve 15, pump 1 and pump 3, adjust the flow meter 16, and deliver the reaction material liquid to the phase separator 21 at a flow rate of 100L / h, so that the pump 1 and pump 3...

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Abstract

The invention discloses a preparation method of high-grade 4-tert-butylbenzaldehyde and a preparation apparatus of high-grade 4-tert-butylbenzaldehyde. The preparation method of high-grade 4-tert-butylbenzaldehyde comprises the following steps: A) 4-tert-butylbenzaldehyde, water and a catalyst without halogen are mixed in a micrometer bubble reactor for carrying out an oxidation reaction, in order to obtain reaction feed liquid; B) oil-water separation is carried out for reaction feed liquid in order to obtain water phase and oil phase, water phase contains the catalyst, and the oil phase contains 4-tert-butylbenzaldehyde and impurities; and C) 4-tert-butylbenzaldehyde and the impurities are separated in order to obtain high-grade 4-tert-butylbenzaldehyde. 4-tert-butylbenzaldehyde prepared by the preparation method of high-grade 4-tert-butylbenzaldehyde according to an embodiment does not contain halogen, and can be applied to the fields of foodstuff, medicine, perfume and the like.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for preparing high-grade p-tert-butylbenzaldehyde, and also to a device for preparing high-grade p-tert-butylbenzaldehyde. Background technique [0002] High-grade p-tert-butylbenzaldehyde refers to halogen-free p-tert-butylbenzaldehyde. High-grade p-tert-butylbenzaldehyde can be used in medicine, food, spices and other fields. The domestic production of p-tert-butylbenzaldehyde mainly adopts the process of chlorination and hydrolysis of p-tert-butyltoluene, which leads to cumbersome production process and serious pollution due to the use of chlorine gas, and the residual chlorine in the product cannot be completely removed, so it is difficult to be used in food and medicine field. Using acetic acid as a solvent and Co / Mn / Br as a catalyst to catalyze the oxidation of p-tert-butyltoluene is one of the research hotspots in the synthesis of p-tert-butylbenzaldehyde. This method c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/36C07C47/542
CPCC07C45/36C07C47/542
Inventor 巫先坤张锋戴建军周腾腾
Owner NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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