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Preparation method of antioxidant BHT

A technology of antioxidants and synthesis methods, applied in the preparation of organic compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., to improve thermal stability, improve preparation efficiency, and promote catalytic activity Effect

Inactive Publication Date: 2018-07-17
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to conduct in-depth research on the above-mentioned prior art, thereby providing a new synthesis method of antioxidant BHT, which adopts the nickel-doped activated alumina solid prepared by the sol-gel method The catalyst not only has a relatively low reaction temperature and high catalytic activity, but its biggest advantage lies in its high selectivity to BHT and continuous reaction, which greatly improves production efficiency and simplifies subsequent separation steps

Method used

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  • Preparation method of antioxidant BHT
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Experimental program
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Effect test

Embodiment 1-18

[0032] The method of preparing a nickel-doped activated alumina solid catalyst by the sol-gel method is as follows: Weigh a calculated amount of nickel compound and group VIII transition metal salt compound into ethylene glycol / butanol, and then add it to ethylene glycol / butanol at room temperature. Aluminum isopropoxide is added to the continuously stirred solution, and the resulting solution is allowed to stand and age for 24 to 120 hours. The obtained gel is evaporated and concentrated. A ball mill is used to prepare pellets with a diameter of 1 to 2 mm. After drying at room temperature, they are dried at 110 to 120°C for 12 to 36 hours, and then calcined in air at 400 to 600°C for 4 to 6 hours. .

[0033] Weigh 15g each of the nickel-doped activated alumina catalysts CUI-1~CUI-18 prepared by the sol-gel method in batches and fill them in the constant temperature section of the fixed bed reactor, and fill both ends of the catalyst bed Inert magnetic ball. The reactor is divi...

Embodiment 19-24

[0037] Weigh 15g of CUI-16 and fill it in the constant temperature section of the fixed bed reactor. The two ends of the catalyst bed are filled with inert magnetic balls. The reactor is divided into four sections for temperature control. There is a built-in thermocouple in the middle of the reactor for real-time Monitor the actual temperature at each point of the catalyst bed. Before the reaction, the temperature of the gasification chamber was gradually increased to 350°C under nitrogen flow, and the temperature of the catalyst bed was gradually increased to 230-260°C. After reaching the set temperature, continue to purge with nitrogen for 0.5 hours. The p-cresol is melted by heating with a heating belt, and then the mass space velocity is controlled to 0.1~2h with a syringe pump -1 . The isobutylene corresponding to 1:1~1:3 molar equivalent is delivered to the gasification chamber with a volume mass flow meter. After the p-cresol is gasified in the gasification chamber, it...

Embodiment 25

[0041] Using the catalyst CUI-16, change isobutylene to tert-butanol according to the experimental method in the above examples, control the molar ratio of tert-butanol to p-cresol to 2.8, mix tert-butanol and p-cresol evenly, and then inject the sample. The temperature of the layer was controlled at 260°C, and after two hours of continuous reaction, the samples were taken within 15 minutes and analyzed by gas chromatography. The conversion rate of p-cresol was 81% and the selectivity of BHT was 82%.

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Abstract

The invention discloses a method for synthesizing antioxidant BHT. Among current synthetic methods, some methods are highly corrosive to equipment, some methods are high in three wastes, and some methods cannot continuously produce, are low in synthesis efficiency, and are not conducive to industrialization. The method utilizes p-cresol and isobutylene as raw materials, and conducts catalytic reactions in a nickel-doped active aluminium oxide solid catalyst prepared by a sol-gel method, the structure of the active aluminium oxide catalyst is Ni&X@Al2O3, and the weight ratio of the nickel is 0.2-10%; the X is a VIII-group transition metal other than the nickel, and the content of the X is less than the nickel. When synthesizing target products, the method has the advantages of easy control,green environmental protection, long catalyst life, high stability, continuous production and convenient industrialization.

Description

Technical field [0001] The invention belongs to the field of preparation of fine chemicals, and specifically relates to a synthesis process of an antioxidant BHT. Background technique [0002] Antioxidant BHT, also called antioxidant 246, is called di-tert-butylhydroxytoluene in English, and its chemical name is 2,6-di-tert-butyl-p-cresol, and its molecular formula is C 15 H 24 O, the molecular weight is 220.35, and the CAS number is 128-37-0. The chemical molecular structure of antioxidant BHT is as follows: [0003] [0004] Antioxidant BHT is an excellent general-purpose phenolic antioxidant. It is non-toxic, non-flammable, non-corrosive, and has good storage stability. It can inhibit or delay the oxidative degradation of plastic or rubber and prolong its service life. Appearance is white or light yellow crystalline powder, soluble in solvents such as benzene, toluene, methanol, ethanol, acetone, acetic acid, and petroleum ether, but insoluble in water. It is an excellent anti...

Claims

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Application Information

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IPC IPC(8): C07C37/14C07C39/06B01J23/89B01J23/755
CPCC07C37/14B01J23/755B01J23/892C07C39/06
Inventor 肖唐鑫徐丽湘仲伟伟周玲
Owner CHANGZHOU UNIV
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