Method for removing water in anisole by using loaded type calcium oxide water removing agent

A load-type, calcium oxide technology, applied in ether preparation, organic chemistry, ether separation/purification, etc., can solve the problems of anisole loss, poor water removal effect, and inability to guarantee anisole water content, etc.

Active Publication Date: 2016-02-03
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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Problems solved by technology

However, the loss of anisole in the gas stripping process is serious, and the energy consumption is large; with 3A, 4A molecular sieves as adsorbent, the water content of anisole after adsorption is about 25ppm, and this method cannot guarantee that the water content in anisole is low In 20ppm; Membrane separation method is not yet documented in the field of anisole water removal, bibliographical reports prepare absolute ethanol with hollow fiber membrane separation method, and the water content in the gained ethanol product is as high as 2000ppm, and dehydration effect is not good

Method used

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[0028] 1. The raw materials used are calcium oxide solid, industrial anisole, nitrogen, aluminum hydroxide solid, high-purity silicon powder, and inert gas. Fixed bed reactor, high pressure advection pump, muffle furnace, disc ball forming machine, drying oven, Karl Fischer trace moisture analyzer (SF101 type, sensitivity 0.1ugH2O, measuring range: 0.1ug-200mgH 2 O) etc.

[0029] 2. Preparation of water-removing agent: Silica sol was prepared by sol-gel method using high-purity silica powder as raw material under alkaline conditions. Take 350ml of this silica gel and put it into a drying oven, adjust the temperature of the drying oven to keep the temperature of the drying oven at 80°C. Dry the silica sol for 10-15 hours. After the silica sol loses water and condenses into a block, take about 50g of the silica sol that has dehydrated and condensed into a block and put it in a muffle furnace. ℃ for 10 hours, after natural cooling, take out the fired sample, grind the sample in...

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Abstract

The invention provides a method for removing water in anisole by using a loaded type calcium oxide water removing agent and relates to an industrial anisole water removing method. The method is characterized by comprising the following steps: filling the loaded type calcium oxide water removing agent into a fixed-bed reactor and pumping anisole liquid containing trace amount of water by using a high-pressure pump; controlling a reaction temperature to be 25 to 160 DEG C to react; by using a CaO+H2O=Ca(OH)2 chemical reaction, finally obtaining an anhydrous anisole solution, wherein the content of the anisole in raw materials is 70 percent to 99 percent and the mass percent of calcium oxide in the loaded type calcium oxide water removing agent is 5 percent to 30 percent. With the adoption of the method, a bottleneck problem of the trace amount of water in the anisole to a boron isotope separation industrial production process is solved; meanwhile, influences that a pasty calcium hydroxide product generated on the outer surface in a calcium oxide water removing process covers calcium oxide and a water removing reaction is not continuously carried out are avoided, and the calcium oxide water removing efficiency is improved.

Description

technical field [0001] The invention relates to a method for removing moisture in anisole, in particular to a method for removing moisture in anisole by using a loaded calcium oxide water remover. Background technique [0002] Anisole is an important organic compound that can be used as a solvent, fragrance, insect repellant, etc. At present, anisole is widely used as an industrial boron trifluoride chemical exchange distillation method to produce boron 10 (B 10 ) in the use of complexing agents. This method relies on boron trifluoride (BF 3 ) and complexing agent to form a complex to produce B 10 . At low temperature, BF 3 Both can undergo complexation reaction with anisole, and with the increase of temperature, B 11 f 3 It is easier to separate from the cleavage of the anisole boron trifluoride complex, so that the B 10 f 3 Enriched in anisole to separate B 10 the goal of. For other ethers as complexing agent production B 10 Among the methods, the exchange dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/36C07C43/205
CPCC07C41/36C07C43/205
Inventor 石磊姚杰赵佳
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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