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A kind of synthetic method of rubidium extractant 4-ethyl-2 (alpha-methylbenzyl) phenol

A synthesis method, methylbenzyl technology, applied in the field of new mesoporous molecular sieve PW12/Fe-Al-MCM-41 catalyst, can solve the problems of many by-products, corrosion equipment, difficult separation, etc.

Inactive Publication Date: 2016-04-06
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the sulfuric acid, phosphoric acid, AlCl used in this reaction 3 , FeCl 3 and other liquid catalysts, resulting in many unfavorable factors such as corrosion of equipment, low product yield, many by-products, and difficult separation, and the cost remains high

Method used

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  • A kind of synthetic method of rubidium extractant 4-ethyl-2 (alpha-methylbenzyl) phenol
  • A kind of synthetic method of rubidium extractant 4-ethyl-2 (alpha-methylbenzyl) phenol
  • A kind of synthetic method of rubidium extractant 4-ethyl-2 (alpha-methylbenzyl) phenol

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Prepare Al-MCM-41 by hydrothermal method, the molar ratio of raw materials is:

[0018] NaAlO 2 :TEOS:CTAB:NaOH:H 2 O=0.1:1:0.2:0.5:100. 7.2gCTAB was dissolved in 180mL of deionized water, heated and stirred to make it dissolve into a transparent solution, and aluminum source (0.82g sodium aluminate), silicon source ( 20.83g ethyl orthosilicate), sodium hydroxide 2.0g, make it mix evenly, continue to stir for 2h; adjust the pH of the solution to about 10.5 with 2mol / L sulfuric acid solution, continue to stir for 1h to form a uniform gel phase, and then It was moved into a stainless steel reaction kettle lined with polytetrafluoroethylene, and hydrothermally crystallized at 150°C for 48 hours; the product after crystallization was filtered, washed with water, dried, and the temperature was programmed to 550°C to be roasted to remove the template agent. Add 0.5gAl-MCM-41 to the solution containing 0.001mol / LFeCl 3 ·6H 2 O and 0.05g of ammonium phosphotungstate in 100m...

example 2

[0020] Slowly drop 10.4g of styrene into the PW with 36.4g of p-ethylphenol and 6.5g of silicon-aluminum ratio (molar ratio) of 10 12 / Fe-Al-MCM-41 mesoporous molecular sieve catalyst and 100mL cyclohexane in a 250mL three-neck reaction flask, reflux at 80°C for 4h, stop the reaction, cool to room temperature, filter and separate the reaction liquid and solid molecular sieve catalyst, and distill off the solvent under reduced pressure cyclohexane to obtain 45.82 g of light yellow transparent liquid. The product was purified by silica gel column chromatography, ethyl acetate and petroleum ether were used as developing solvents (V (petroleum ether): V (ethyl acetate) = 40:1) for separation and purification, and the effluent was collected for detection by TLC. The same effluents were combined, and the petroleum ether and ethyl acetate in the effluents were distilled off under reduced pressure to obtain 18.42 g of a light yellow viscous main product and 1.365 g of a yellow solid b...

example 3

[0022] Slowly drop 104.1lg of styrene into the PW with 364.5g of p-ethylphenol and 65g of silicon-aluminum ratio (molar ratio) of 10 12 / Fe-Al-MCM-41 molecular sieve catalyst and 1000mL cyclohexane in a 2500mL three-necked reaction flask, reflux at 75°C for 4h, stop the reaction, cool to room temperature, filter and separate the reaction liquid and solid molecular sieve catalyst, and distill off the solvent cyclohexane under reduced pressure alkane to obtain 452.6 g of light yellow transparent liquid. The product was purified by silica gel column chromatography, ethyl acetate and petroleum ether were used as developing solvents (V (petroleum ether): V (ethyl acetate) = 40:1) for separation and purification, and the effluent was collected for detection by TLC. The same effluents were combined, and the petroleum ether and ethyl acetate in the effluents were distilled off under reduced pressure to obtain 182.4 g of a light yellow viscous main product and 12.68 g of a light yellow...

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Abstract

The invention relates to a synthesis method of a new extraction agent 4-ethyl-2 (α-methylbenzyl)phenol for the separation of rubidium and potassium and a preparation method of a catalyst required for the synthesis. Using styrene and p-ethylphenol as raw materials and PW12 / Fe-Al-MCM-41 new mesoporous molecular sieve as catalyst, 4-ethyl-2 (α-methylbenzyl)phenol was synthesized. Mesoporous molecular sieve Al-MCM-41 was prepared using a hydrothermal method and part of the Al in the molecular sieve framework was replaced by heteropolyacid active groups such as Fe3+ and phosphotungstic acid through ion replacement to prepare PW12 / Fe-Al-MCM-41 molecular sieve. The yield of 4-ethyl-2(α-methylbenzyl)phenol reaches more than 80%, the selectivity of the main product is greater than 95.0%, and the purity of the product after separation and purification is greater than 95%. A rubidium-potassium separation test was conducted using 4-ethyl-2(α-methylbenzyl)phenol as the extraction agent. The single-stage extraction rate of rubidium was greater than 80%, and the rubidium-potassium separation coefficient reached more than 30.

Description

technical field [0001] As a rare alkali metal element, rubidium has great economic and strategic significance. There are rich rubidium resources in salt brine in my country. Because rubidium coexists with the alkali metal element potassium with very similar properties, the extraction technology of rubidium is extremely difficult. Therefore, new rubidium separation materials are developed to improve the utilization of rubidium in my country's rich brine resources. rate, can bring substantial economic and social benefits. At present, it is mainly used in the extraction and separation of rubidium to replace phenolic extractants. By modifying the structure of phenolic extractants, it is expected to improve the extraction selectivity of rubidium and improve the separation effect. The invention relates to the preparation of a novel mesoporous molecular sieve PW with high catalytic activity and high selectivity 12 / Fe-Al-MCM-41 catalyst, and using the catalyst to establish a new rub...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/14C07C39/15B01J31/28
CPCC07C37/14B01J27/188B01J29/045B01J35/19C07C39/15
Inventor 安莲英黄正根赵先银
Owner CHENGDU UNIVERSITY OF TECHNOLOGY