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Preparation method and preparation system of ethylene glycol (OD) 2

A preparation system and ethylene glycol technology, applied in the field of preparation of ethylene glycol 2, can solve the problems of harsh reaction conditions, expensive catalysts, complicated processes, etc., and achieve the effects of improving conversion rate, low cost, simple and controllable process

Active Publication Date: 2021-03-05
四川新火炬化工有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide ethylene glycol (OD) Preparation method and preparation system, to solve the harsh reaction conditions, complex process, expensive catalyst and difficult separation in the preparation of ethylene glycol (OD) in the prior art and other technical issues

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  • Preparation method and preparation system of ethylene glycol (OD) 2
  • Preparation method and preparation system of ethylene glycol (OD) 2

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preparation example Construction

[0042] Ethylene glycol (OD) of the present invention The first embodiment of the preparation method comprises the following steps:

[0043] (1) Reacting the mixture containing heavy water and ethylene glycol at 100-300° C. under normal pressure for 1-8 hours to generate a first reaction solution containing ethylene glycol (OD) 2 .

[0044] Among them, the reaction temperature is preferably 100-150° C., and the reaction time is preferably 3-5 h.

[0045] The mixture is composed of heavy water with concentration≥99.8% and ethylene glycol with concentration≥99.5%, and the volume ratio of ethylene glycol and heavy water is (1-10):1, preferably (1-3):1.

[0046] (2) Carry out rectification to the first reaction liquid, collect the non-vaporized phase in the first reaction liquid, promptly obtain containing ethylene glycol (OD) 2 The second reaction liquid; Simultaneously, collect the gasified phase An adsorbent is used to absorb the residual ethylene glycol and ethylene glycol (OD...

Embodiment 1

[0072] In the mixer 100 , 1.5 liters of ethylene glycol and 1.5 liters of heavy water (the volume ratio of ethylene glycol and heavy water is 1:1) were pre-mixed first, and the mixture obtained after mixing evenly was input into the reaction tower 200 . The mixture in the reaction tower 200 was reacted at 100° C. to 150° C. under normal pressure for 4 hours to obtain a first reaction liquid. The first reaction liquid enters the primary rectification tower 310 with a top temperature of 40°C to 50°C and continues to rectify for 10 hours to collect the ungasified phase to obtain the second reaction liquid, collect the gasified phase and use activated carbon Adsorption of residual ethylene glycol and ethylene glycol (OD)2 yields dilute heavy water. The second reaction solution was distilled under reduced pressure in a distillation tower 400 with a top temperature of 90-110° C. to obtain 1.2 kg of ethylene glycol (OD) 2 product, and the purity of ethylene glycol (OD) 2 in the produ...

Embodiment 2

[0074] In the mixer 100 , 1.5 liters of ethylene glycol and 4.5 liters of heavy water (the volume ratio of ethylene glycol and heavy water is 1:3) were pre-mixed first, and the mixture obtained after mixing evenly was input into the reaction tower 200 . The mixture in the reaction tower 200 was reacted at 100° C. to 150° C. under normal pressure for 4 hours to obtain a first reaction liquid. The first reaction liquid enters the primary rectification tower 310 with a top temperature of 40°C to 50°C and continues to rectify for 10 hours to collect the ungasified phase to obtain the second reaction liquid, collect the gasified phase and use activated carbon Adsorption of residual ethylene glycol and ethylene glycol (OD)2 yields dilute heavy water. The second reaction solution was distilled under reduced pressure in a distillation tower 400 with a top temperature of 90-110° C. to obtain 1.8 kg of ethylene glycol (OD) 2 product, and the purity of ethylene glycol (OD) 2 in the produ...

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Abstract

The invention discloses a preparation method and preparation system of ethylene glycol (OD) 2. The preparation method of ethylene glycol (OD) 2 comprises the following steps: (1), reacting a mixture containing heavy water and ethylene glycol to generate a first reaction solution containing ethylene glycol (OD) 2; and (2), heating the first reaction solution, and collecting an ungasified phase in the first reaction solution to obtain a second reaction solution containing ethylene glycol (OD) 2. The system for preparing ethylene glycol (OD) 2 comprises: a reaction unit for reacting a mixture containing heavy water and ethylene glycol and outputting a first reaction solution containing ethylene glycol (OD) 2 and a separation unit used for treating the first reaction solution, collecting an ungasified phase and outputting a second reaction solution containing ethylene glycol (OD) 2. The method has the advantages of stable product quality, mild reaction conditions, simple and controllable process and high safety, effectively improves the conversion rate of the raw materials and the yield of the product, and is low in cost and suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to the technical field of ethylene glycol (OD)2, in particular, to a preparation method and a preparation system of ethylene glycol (OD)2. Background technique [0002] Ethylene glycol (OD) 2, the English name is 1,2-Ethanediol-d2 (9CI) or Ethylene glycol-(OD) 2, CASNO (the registration number formulated by the American Chemical Abstracts Service for chemical substances, CAS is Chemical Abstracts Service Abbreviation) is: 2219-52-5, the structural formula is (CH2OD)2, which is an important chemical raw material, intermediate and refrigerant. In chemical synthesis, it is a commonly used NMR solvent and reagent, widely used in laboratory research work. [0003] Since the activity of deuterium gas is significantly lower than that of hydrogen gas, all or part of the hydrogen atoms in ethylene glycol will be replaced by the ordinary ethylene glycol preparation method, and there are problems such as harsh reaction conditions, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/00C07C29/76C07C29/80C07C31/20C07B59/00
CPCC07C29/00C07C29/76C07C29/80C07C31/202C07B59/001C07B2200/05Y02P20/52
Inventor 翁贵萍钱永中陈圳源邓奎李鹰王洪飞袁真才
Owner 四川新火炬化工有限责任公司