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A kind of method for preparing p-tert-butylbenzaldehyde by liquid-phase oxidation of p-tert-butyltoluene

A technology of p-tert-butyltoluene and p-tert-butyl, which is applied in the chemical field, can solve problems such as affecting mass transfer, increasing equipment investment, and hidden safety hazards, achieving the effects of mild reaction conditions, reducing investment costs, and improving quality

Active Publication Date: 2021-09-28
NANJING UNIV YANCHENG ENVIRONMENTAL PROTECTION TECH & ENG RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When water is used as the reaction solvent, due to the poor mutual solubility between p-tert-butyltoluene and the solvent, it affects the mass transfer between the gas-liquid two phases. In order to strengthen the mass transfer, the reaction is usually carried out at a higher reaction pressure, which not only It will increase equipment investment, and there are certain security risks

Method used

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  • A kind of method for preparing p-tert-butylbenzaldehyde by liquid-phase oxidation of p-tert-butyltoluene
  • A kind of method for preparing p-tert-butylbenzaldehyde by liquid-phase oxidation of p-tert-butyltoluene

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Effect test

Embodiment 1

[0034] Weigh 1.48 kg of p-tert-butyl toluene and place it in a raw material storage tank, weigh 1.41 kg of water, 0.007 kg of p-tert-butyl benzoate, 0.063 kg of tert-butyl benzyl alcohol, 15 mg of auxiliary agent, 15 mg of catalyst, and over Sodium oxycarbonate 0.0015kg is dissolved in the solvent storage tank, wherein the additives are 10 mg of sodium p-tert-butylbenzoate and 5 mg of sodium dodecylbenzenesulfonate, and the catalyst is benzopyrimidine cobalt complex, through the corresponding metering pump Transport to the corresponding storage tank, heat up to 40°C through the heat exchanger, the two fluids collide in the impingement flow reactor, and the micron-sized emulsion produced is transported to the bubble column reactor through the ejector, and the ejector entrains and bubbles Oxygen and fresh oxygen at the top of the reactor are oxidized in the bubble column reactor, and oxygen is delivered to the bubble reactor through the gas distributor to ensure the reaction for ...

Embodiment 2

[0036] Take by weighing 1065g of p-tert-butyl toluene and place it in a raw material storage tank, weigh 7.1 kg of water, 460 g of p-tert-butyl benzoate, 1.42 kg of p-tert-butyl benzyl alcohol, 0.4 g of auxiliary agent, 0.4 g of catalyst, and over Sodium oxycarbonate 480g is dissolved in the solvent storage tank, wherein auxiliary agent is 0.1 g of sodium p-tert-butylbenzoate, 0.1 g of potassium p-tert-butylbenzoate and 0.2 g of heavy alkylbenzene sulfonate, and the catalyst is nickel benzopyrazole 0.2 g of the complex and 0.2 g of the benzopyridine vanadium complex were transported to the corresponding storage tank through the corresponding metering pump, and the temperature was raised to 80°C through the heat exchanger, and the two fluids collided in the impinging flow reactor, resulting in The micron-sized emulsion is transported to the bubble column reactor through the ejector, and the oxygen and fresh oxygen at the top of the bubble reactor are entrained by the ejector, an...

Embodiment 3

[0038] Take by weighing 1.48 kg of p-tert-butyltoluene and place it in a raw material storage tank, weigh 9.99 kg of water, 1.131 kg of p-tert-butyl benzoate, 114 g of p-tert-butyl benzyl alcohol, 0.103 g of auxiliary agent, 0.5 g of catalyst, and pro-oxidant Sodium percarbonate 0.069 kg is dissolved in the solvent storage tank, wherein the additives are 0.05 g of lithium p-tert-butylbenzoate, 0.0.5 g of potassium p-tert-butylbenzoate and 0.003 g of heavy alkylbenzenesulfonate, and the catalyst is 0.2 g of benzopyrazole aluminum complex and 0.3 g of benzopyridine copper complex are transported to the corresponding storage tank through the corresponding metering pump, and the temperature is raised to 60 °C through the heat exchanger. Internal collision, the micron-sized emulsion produced is transported to the bubble column reactor through the injector, and the injector entrains the oxygen and fresh oxygen at the top of the bubble reactor, and the oxidation reaction is carried ou...

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Abstract

The invention discloses a method for preparing p-tert-butylbenzaldehyde by liquid-phase oxidation of p-tert-butyltoluene. The method includes (1) preheating p-tert-butyl toluene and reaction solvent mixture and mixing them in an impingement flow reactor to form a micron-sized emulsion; (2) passing the micron-sized emulsion into a bubble column reactor through an injector The reaction feed liquid is obtained after internal reaction with oxygen; (3) the reaction feed liquid is subjected to oil-water separation to obtain an oil phase and a water phase; (4) the oil phase is separated to obtain the product p-tert-butylbenzaldehyde; wherein , containing p-tert-butylbenzoate, p-tert-butylbenzyl alcohol, water, catalyst, auxiliary agent and auxiliary oxidant in the reaction solvent mixture. The invention has the advantages of high selectivity to p-tert-butylbenzaldehyde, mild reaction conditions, recyclable catalysts, auxiliary agents and solvents, green and pollution-free.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of p-tert-butylbenzaldehyde. Background technique [0002] 4-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 can improve the selectivity of p-tert-butylbenzaldehyde, but due to the use of Bromide, a small amount of bromine element will inevitably remain in the product, which ...

Claims

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Application Information

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Patent Type & Authority Patents(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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