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A kind of preparation technology of dioxolane

A technology for the preparation of dioxolane, which is applied in the direction of sustainable manufacturing/processing, chemical industry, membranes, etc., can solve problems such as high pressure, high equipment requirements, and waste water generation, and reduce the probability of coking and inactivation. High strength and high separation selectivity

Active Publication Date: 2019-02-15
杨河峰 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high pressure in the tower, high requirements for equipment, and a large amount of waste water is generated.

Method used

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  • A kind of preparation technology of dioxolane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Such as figure 1 As shown, a preparation process of dioxolane includes a catalytic reaction process, a membrane separation and dehydration process, and a rectification process.

[0046] The specific operation is as follows:

[0047] a. Open the ethylene glycol material pump 3 first, send the ethylene glycol in the ethylene glycol storage tank 1 into the pre-reactor 6 after being heated by the heat exchanger 5, open the formaldehyde material pump 4 at the same time, and put the formaldehyde storage tank 2 The 37% formaldehyde solution in the mixture is heated by the heat exchanger 5 and then sent to the pre-reactor 6 to control the flow rate of the material pump, keep the feed volume ratio of formaldehyde and ethylene glycol at 1:1, and control the temperature in the pre-reactor The temperature is 80°C, the pressure is 0.2Mpa, and the pre-reaction is carried out under the action of a catalyst;

[0048] b. After the pre-reaction, the content of 66% dioxolane and unreact...

Embodiment 2

[0060] The specific operation is as follows:

[0061] a. Open the ethylene glycol material pump 3 first, send the ethylene glycol in the ethylene glycol storage tank 1 into the pre-reactor 6 after being heated by the heat exchanger 5, open the formaldehyde material pump 4 at the same time, and put the formaldehyde storage tank 2 The 40% formaldehyde solution in the solution is sent into the pre-reactor 6 after being heated by the heat exchanger 5, the flow rate of the material pump is controlled, the feed volume ratio of formaldehyde and ethylene glycol is kept at 1.5:1, and the temperature in the pre-reactor is controlled. The temperature is 90°C, the pressure is 0.12Mpa, and the pre-reaction is carried out under the action of the catalyst;

[0062] b. After the pre-reaction, the content of 62% dioxolane and unreacted formaldehyde and ethylene glycol are sent to the middle part of the catalytic rectification tower 7, the catalytic rectification tower reboiler 8 is opened, and...

Embodiment 3

[0074] The specific operation is as follows:

[0075] a. Open the ethylene glycol material pump 3 first, send the ethylene glycol in the ethylene glycol storage tank 1 into the pre-reactor 6 after being heated by the heat exchanger 5, open the formaldehyde material pump 4 at the same time, and put the formaldehyde storage tank 2 The 40% formaldehyde solution in the solution is sent into the pre-reactor 6 after being heated by the heat exchanger 5, the flow rate of the material pump is controlled, the feed volume ratio of formaldehyde and ethylene glycol is kept at 1.8:1, and the temperature in the pre-reactor is controlled. The temperature is 100°C, the pressure is 0.05Mpa, and the pre-reaction is carried out under the action of a catalyst;

[0076] b. After the pre-reaction, the content of 60% dioxolane and unreacted formaldehyde and ethylene glycol are sent to the middle part of the catalytic rectification tower 7, the catalytic rectification tower reboiler 8 is opened, and ...

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Abstract

The invention discloses a preparation technology of dioxolame, belongs to the field of downstream deep processing of ethylene glycol, and is applied to multiple fields of lithium batteries, refining chemical engineering intermediates, synthesis materials, electronic chemicals and the like. The preparation technology specifically comprises the following steps of reacting formaldehyde and ethylene glycol in a pre-reactor, and sending into a catalyzing and rectification tower to perform catalytic reaction and rectification, so as to obtain dioxolame with purity of 93.5 to 94.5% at the top of the tower; dewatering and separating a tower top discharged material by molecular sieve membrane equipment, so as to reach the product purity of 95.0 to 99.0%; separating by a rectification tower, so as to obtain a dioxolame product with purity of 99.9%. The preparation technology has the advantages that the separation technology includes three parts, i.e., a prereaction-catalyzing and rectification tower system, a molecular sieve membrane system and a common-pressure rectification system, so that the technology process is shortened, and the energy consumption is decreased; the integration property is strong, the normal-running traditional technology is properly modified, the investment is little, the running cost is reduced, and the preparation technology is suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of dioxolane, in particular to a novel production process of dioxolane. Background technique [0002] Dioxolane, its molecular formula: C3H6O2, pure product is a colorless transparent liquid, widely used in solvents, detergents, extractants: it can be used as a detergent for metal films; PVC, cellulose derivatives and other polymers Solvents for paints and adhesives; components of photosensitive solutions and developer solutions; extractants for oils, waxes, medicines (vitamins, etc.); solvents for lithium battery electrolytes, etc. [0003] Dioxolane is mainly prepared by cyclization reaction of ethylene glycol and formaldehyde in the presence of acid catalysts such as sulfuric acid, trifluoroboric acid, solid acid and heteropoly acid. Pure dioxolane is typically isolated from the reaction mixture by distillation or rectification. [0004] The earliest patent report (West German patent 1914209) obtained 1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/12B01D71/38B01D69/02B01D67/00
CPCB01D67/0079B01D69/02B01D71/38B01D2325/24B01D2325/36C07D317/12Y02P20/10Y02P20/50
Inventor 杨河峰孙超
Owner 杨河峰