Chromatographically pure ethyl ether and preparation method and production system thereof

A kind of chromatographically pure, ether technology

Inactive Publication Date: 2017-12-22
HUBEI ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chromatographically pure ether is one of the commonly used mobile phases for liquid chromatography, and its domestic chromatographically pure market is mostly monopolized by foreign reagent companies, such as Merck, Sigma, Fisher, Tedia, etc. Their products are expensive, compared to chromatographically

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  • Chromatographically pure ethyl ether and preparation method and production system thereof
  • Chromatographically pure ethyl ether and preparation method and production system thereof

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preparation example Construction

[0027] The embodiment of the present invention provides a preparation method of chromatographically pure ether, which comprises:

[0028] S1. Using industrial grade diethyl ether as a raw material, carry out oxidation removal and neutralization reaction to obtain a reaction solution.

[0029] Colorless transparent liquid. Has a special pungent smell. with sweetness. Very volatile. Its vapor is heavier than air. Under the action of air, it can be oxidized to peroxide, aldehyde and acetic acid, and its oxidation can be promoted by exposure to light. Oxidation and impurity removal of industrial grade ether is to mix industrial grade ether with alkali and potassium permanganate. Preferably, the base includes at least one of sodium hydroxide, potassium hydroxide and calcium hydroxide. Potassium permanganate can oxidize impurities such as alcohols, aldehydes, and ketones mixed in industrial grade ether into carboxylic acids, and carboxylic acids and alkalis react to form salts...

Embodiment 1

[0054] Present embodiment 1 provides a kind of production system 100 of chromatographically pure ether, with reference to figure 1 As shown, it includes: a reaction kettle 110 , a mixer 131 , a 4A molecular sieve column 132 , a calcium hydride column 133 , a basic alumina column 134 , an activated carbon adsorption column 135 , a rectification tower 140 and a circulation pump 120 .

[0055] Among them, the mixer 131 , 4A molecular sieve column 132 , calcium hydride column 133 , basic alumina column 134 , and activated carbon adsorption column 135 are arranged in parallel, and form circulation pipelines with circulation pump 120 and reaction kettle 110 respectively. Further, the input end of the circulation pump 120 is communicated with the liquid phase outlet at the bottom of the reactor 110, and the output end of the circulation pump 120 is respectively communicated with the mixer 131, 4A molecular sieve column 132, calcium hydride column 133, basic alumina column 134, The fe...

Embodiment 2

[0061] The present embodiment provides a kind of chromatographically pure diethyl ether, and its preparation method is as follows:

[0062] S1. Introduce 50L of industrial-grade ether (Jinzhou Petrochemical, purity ≥ 98wt%) raw material in the reactor 110, add 5mol% sodium hydroxide and 5mol% potassium permanganate, open the valve of the mixer 131 and the circulation pump 120 , establish the circulation between the reaction kettle 110, the circulation pump 120 and the mixer 131 until the color of the solution in the reaction kettle 110 no longer changes.

[0063] S2. Open the acid dripping tank 113, let the concentrated sulfuric acid therein drop slowly into the reaction kettle 110, and maintain the circulation for 0.5h.

[0064] S3. Add 50L of water into the reaction kettle 110, maintain the circulation for 0.5h, close the valve of the mixer 131 and the circulation pump 120, and let stand for 3h to make the solution in the reaction kettle 110 layered; remove the lower water l...

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Abstract

Chromatographically pure ethyl ether and a preparation method and a production system thereof relate to the technical field of purification of chemical products. The preparation method is characterized in that industrial ethyl alcohol serves as a raw material and is subjected to oxidation impurity removal and a neutral reaction at first and then 4A molecular sieve adsorption, calcium hydride adsorption, basic alumina adsorption and activated carbon adsorption to obtain a rectifying stock solution, and at last, the rectifying stock solution is rectified. The preparation method is low in production cost, can prepare the chromatographically pure ethyl ether with good quality and high yield, and meets the requirements of chromatographically pure reagents. The production system comprises a 4A molecular sieve column, a calcium hydride column, a basic alumina column and an activated carbon adsorption column which are arranged in parallel and constitute a circulation line with a reaction kettle, and a gas-phase outlet of the reaction kettle is communicated with a gas-phase inlet in the bottom of a rectifying column. The production system is specially used for preparing the chromatographically pure ethyl ether, is high in production efficiency, can obtain the product with high purity, and can realize large-scale industrial production of the chromatographically pure ethyl ether.

Description

technical field [0001] The invention relates to the technical field of purification of chemical products, in particular to a chromatographically pure ether, a preparation method and a production system thereof. Background technique [0002] Chromatographically pure refers to the standard reagents used in chromatographic analysis. Its ultraviolet absorbance at low wavelengths is relatively low. Under chromatographic conditions, only peaks of specified compounds appear, and impurity peaks cannot appear. In addition to the high content, it also has high requirements for fine dust and moisture, which belongs to the category of high-purity reagents. Chromatographically pure ether is one of the commonly used mobile phases for liquid chromatography, and its domestic chromatographically pure market is mostly monopolized by foreign reagent companies, such as Merck, Sigma, Fisher, Tedia, etc. Their products are expensive, compared to chromatographically pure For users, it will lead t...

Claims

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Application Information

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IPC IPC(8): C07C41/34C07C41/36C07C41/42C07C41/44C07C43/06
CPCC07C41/34C07C41/36C07C41/42C07C41/44C07C43/06
Inventor 覃彩芹文胜郑根稳龚春丽赵正崇程凡董浩
Owner HUBEI ENG UNIV
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