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Treatment method of fluorine-containing olefin production waste

A technology for fluorine-containing olefins and waste production, which is applied in the fields of organic chemistry methods, chemical instruments and methods, purification/separation/stabilization of organic compounds, etc. Solvent waste and other problems, to achieve the effect of facilitating industrial scale-up

Active Publication Date: 2020-06-26
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned method can handle the fluorine-containing olefin production waste in the alcohol solvent system, but it cannot handle the waste of the non-alcohol polar solvent, because the non-alcohol polar solvent is easy to Form a stable complex with ZnCl2 and cannot be further separated, such as DMF and ZnCl2 form a stable complex, see the literature Inorg. Chem. 1983, 22, 136-140
[0006] In view of the fact that the existing technology is unable to deal with fluorine-containing olefin production waste using non-alcoholic polar solvents, it is necessary to develop a utilization method for fluorine-containing olefin production waste to Disposal of waste from the preparation of fluoroolefins using non-alcoholic polar solvents

Method used

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  • Treatment method of fluorine-containing olefin production waste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 200 g of 325-mesh zinc powder and 800 g of DMF into a 2L four-necked flask with a mechanical stirrer, a constant-pressure addition funnel, a reflux condensing device, and a thermometer conduit, and add 98.5% of 4,5-dichloro-2,2, Add 500 g of 4-trifluoro-5-trifluoromethoxy-1,3-dioxolane into the constant pressure funnel, start stirring and heating, and start dropping after the internal temperature reaches 80°C. During the dropping process, control The internal temperature is 80-85°C. After the dropwise addition, continue to stir and react at 80°C for 1 hour. The reaction equation is as follows:

[0036]

[0037] The product 2,2,4-trifluoro-5-trifluoromethoxy-1,3-dioxole was collected by an ice-water cold trap. After the reaction was completed, 1135g of the still residue was obtained by DMF, zinc powder and ZnCl 2 composition. The scrap composition is 70.5wt% DMF, 9.3wt% zinc powder and 20.2wt% zinc chloride. Add 250 g of deionized water to the residual liquid of...

Embodiment 2

[0041] Add 300g of water to 1000g of fluorine-containing olefin production waste composed of 55wt% DMF, 12wt% zinc powder and 33wt% zinc chloride, let it stand overnight, recover the lower layer of zinc powder, and obtain 900g of supernatant, add 23% sodium carbonate solution 1550g, ZnCl 2The molar ratio of sodium carbonate to sodium carbonate is 1:1.1, reacted at 60°C, filtered, washed and dried to obtain 287g of basic zinc carbonate. 2523-2016), N.D. in the table means not detected. The filtrate obtained 300g of sodium chloride through evaporation and crystallization, and obtained 512g of DMF with a content of 98.4% after rectification under reduced pressure, and the recovery rate of DMF was 91.6%.

[0042] Table 1 Analytical data of basic zinc carbonate

[0043] Zinc content moisture content Ignition weight loss Manganese (mg / kg) Copper (mg / kg) Cadmium (mg / kg) Lead (mg / kg) Iron (mg / kg) 57.85% 1.48% 25.92% 15.6 1.9 N.D. N.D. 20.0

...

Embodiment 3

[0048] Add 300g of water to 1000g of fluorine-containing olefin production waste composed of 55wt% DMF, 12wt% zinc powder and 33wt% zinc chloride, obtain 102g of zinc powder after centrifugal filtration, add 1420g of 35% potassium carbonate solution to the filtrate, ZnCl 2 The molar ratio with potassium carbonate is 1:1.2, react at 60°C, filter, wash and dry to obtain 280g of basic zinc carbonate. The filtrate was evaporated and crystallized to obtain 491 g of potassium chloride, and the analytical data of potassium chloride are shown in the table below. Obtain 495g of DMF with a content of 99.4% after rectification under reduced pressure, and the DMF recovery rate is 89.5%.

[0049] Table 2 Potassium chloride analysis data

[0050] Calcium (mg / kg) Magnesium (mg / kg) Iron (mg / kg) Potassium chloride (g / 100g) 47.8 3 1.92 98.4

[0051] Using CF 3 OCFCl-CF 2 The reaction between Cl and zinc powder verifies the performance of recovered zinc powder.

...

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Abstract

The invention discloses a method for treating fluorine-containing olefin production waste, which is particularly suitable for a dechlorination system taking metal zinc as a dechlorinating agent and anon-alcohol polar organic solvent as a solvent. The method comprises the following steps: dissolving zinc chloride, carrying out solid-liquid separation, carrying out a double decomposition reaction,filtering, washing, drying, carrying out evaporative crystallization and rectifying. The method is used for comprehensively treating the fluorine-containing olefin production waste, and all componentsin the waste are treated.

Description

technical field [0001] The invention relates to a treatment method for chemical waste, in particular to a treatment method for fluorine-containing olefin production waste. Background technique [0002] Fluorinated olefins are a class of industrially important chemical intermediates, which are usually prepared by reacting chlorofluoroalkane precursors with metal dechlorination agents in organic solvents. The solvent used in the reaction is usually a polar solvent, which is mainly divided into two categories: alcoholic solvents and non-alcoholic polar solvents. Generally speaking, alcohols (such as methanol, ethanol, isopropanol, etc.) are used as solvents for simple fluorine-containing olefins such as chlorotrifluoroethylene and difluorodichloroethylene. More complex fluorine-containing olefins such as perfluoromethyl vinyl ether, perfluorosulfonyl fluoride vinyl ether, 2,2,4-trifluoro-5-trifluoromethoxy-1,3-dioxa Non-alcoholic polar solvents are often used as cyclopentene,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B63/00C07D307/08C07D207/267C07C253/34C07C255/03C07C231/24C07C233/03C07C233/05C01G9/00
CPCC07B63/00C07D307/08C07D207/267C07C253/34C07C231/24C01G9/00C07C255/03C07C233/03C07C233/05
Inventor 罗凯窦若岸罗生乔陈彬彬甘立兵赖碧红
Owner CHINA BLUESTAR CHENGRAND CO LTD
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