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Method for preparing 4-tert-butyl-2-(alpha-methylbenzyl)phenol

A technology of tert-butylphenol and methylbenzyl, which is applied in the field of polymer compound preparation, can solve the problems of unfavorable industrial production, environmental pollution, low yield, etc., achieve easy large-scale industrial production, and improve the total yield and purity , the effect of reducing production costs

Inactive Publication Date: 2015-01-07
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The traditional solvent synthesis of t-BAMBP has problems such as low yield, many by-products, and difficulty in refining. However, using ionic liquids or heteropolyacids as catalysts not only severely corrodes equipment, but also easily causes environmental pollution, and is not conducive to industrialization. Production

Method used

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  • Method for preparing 4-tert-butyl-2-(alpha-methylbenzyl)phenol
  • Method for preparing 4-tert-butyl-2-(alpha-methylbenzyl)phenol
  • Method for preparing 4-tert-butyl-2-(alpha-methylbenzyl)phenol

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Effect test

Embodiment 1

[0034] Stir 5.0ml of concentrated phosphoric acid (85% by mass) as a catalyst and 6.5ml of phthalic anhydride at room temperature for one hour, stop stirring, add 40.0g of 4-tert-butylphenol, and heat up the oil bath to 110°C When the phenol is completely melted, add 45.0ml of styrene dropwise, keep the drop rate at 1d / s, keep the temperature of the oil bath at 110°C, and raise the system from 110°C to 120°C. After the dropwise addition, the oil bath does not heat up, and the reaction system is heated to 130°C to continue the reaction until the temperature in the system drops slowly, that is, the oil bath is heated to 145°C, and the system is also heated to 145°C, and the reaction is continued for three hours After stopping the reaction. The cooled reaction system was left to stand for separation, and the acid in the lower layer was discarded; the product in the upper layer and the remaining raw materials were directly purified by column chromatography.

[0035] Using petroleum...

Embodiment 2

[0037] Add 100.0ml of concentrated phosphoric acid (85% by mass) and 110.0ml of succinic anhydride into a 500.0ml three-neck flask, put a magnetic stirrer, and react at 50°C. The reaction time is 1.0h, stop the reaction, and proceed directly to the following One step reaction.

[0038] Quickly add 845.0 g of 4-tert-butylphenol into the above mixed acid system from the feeding port, raise the temperature of the system to 110°C while stirring, stop heating the reaction system after the 4-tert-butylphenol is completely melted, and drop Slowly add styrene through the liquid funnel, control the dropping rate to 1d / s, and control the temperature of the system to be basically constant during the dropping process. The amount of styrene added is 905.0ml. After the reaction reaches the end point, cool the reaction system and let it stand for stratification, and use a separatory funnel to completely remove the acid in the lower layer; the upper layer product and the remaining raw materia...

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Abstract

The invention discloses a preparation method of a rubidium / cesium extractant 4-tert-butyl-2-(alpha-methylbenzyl)phenol (t-BAMBP), which comprises the following step: carrying out Friedel-Crafts reaction on raw materials 4-bert-butyl phenol and styrene by using phosphoric acid and acid anhydride as a catalyst to synthesize the 4-tert-butyl-2-(alpha-methylbenzyl)phenol in a simple high-yield mode. The method is characterized in preparation of the catalyst; the phosphoric acid and acid anhydride firstly react under certain conditions to obtain a mixed acid catalyst, and the 4-bert-butyl phenol and styrene are added to react to finally obtain the 4-tert-butyl-2-(alpha-methylbenzyl)phenol at high yield. The product yield of the method can reach 71%, and the product purity is greater than 95%; and the method has the advantages of simple and accessible raw materials, simple synthesis technique, higher product quality and lower production cost.

Description

technical field [0001] The invention belongs to the technical field of polymer compound preparation, and relates to a synthesis process of rubidium and cesium extractant 4-tert-butyl-2-(α-methylbenzyl)phenol. Background technique [0002] The 4-tert-butyl-2-(α-methylbenzyl)phenol (t-BAMBP) of the present invention is a special-effect extractant for rubidium and cesium, and can be used for extracting and separating rubidium and cesium in the lithium mother liquor extracted by lepidolite-lime method , it has good extraction performance, strong selectivity, rapid reaction, and the decontamination coefficient for cesium is greater than 10 6 , The chemical recovery rate of rubidium is greater than 80%. [0003] There are few domestic and foreign literature reports on the synthesis of t-BAMBP, especially its purification process. Kozhevnikov Loading Heteropolyacid H on Mesoporous Molecular Sieves 3 PW 12 o 40 (PW) prepare novel catalyst MCM-41 to be used for catalyzing styren...

Claims

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Application Information

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IPC IPC(8): C07C39/15C07C37/14
CPCC07C37/14C07C39/15
Inventor 蒋历辉邹应萍
Owner CENT SOUTH UNIV
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