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Recovery processing method of 2,7-dichlorofluorene reaction mother solution

A technology for recycling and processing dichlorofluorene acetic acid mother, which is applied in the field of reuse of reaction waste liquid after treatment, can solve problems such as difficult separation, high chlorine activity, easy environmental pollution, etc., and achieves alleviation of environmental pressure, large industrial value, and cost. low cost effect

Inactive Publication Date: 2018-09-28
SHAOXING UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because fluorene has multiple chlorination active sites, and the activity of chlorine gas is high, the selectivity is poor, the yield of this reaction is only about 40%, and a large amount of mother liquor is produced; the mother liquor contains 2-chlorofluorene, 4-chlorofluorene, 2,7-dichlorofluorene, 2,5-dichlorofluorene and 2,4,7-trichlorofluorene and other components are difficult to separate; the previous mother liquor treatment method is: first distill and recover the solvent acetic acid, and then incinerate the residue , due to the large amount of waste and complex components, not only the processing cost is high, but also it is easy to pollute the environment

Method used

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  • Recovery processing method of 2,7-dichlorofluorene reaction mother solution
  • Recovery processing method of 2,7-dichlorofluorene reaction mother solution
  • Recovery processing method of 2,7-dichlorofluorene reaction mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Analytical instruments and equipment used in this example: gas chromatography, MS5973N-GC6890N (Agilent Corporation, USA); nuclear magnetic resonance instrument, AVANCE DMX Ⅱ Ⅰ 400M (TMS internal standard, Bruker Company); high performance liquid chromatography: Agilent Technologies 1200 Series; infrared spectrometer, NICOLET 360FT-IR (Nicolet Instruments, Inc., USA).

[0022] Example 1: Chlorination of fluorene

[0023] Add glacial acetic acid 1200mL, fluorene (I) 166.2g (1 mole) and fluorene (I) into a 2500mL four-necked bottle, maintain the inner temperature at about 40°C and pass in chlorine gas under mechanical stirring, and perform high-performance liquid chromatography to track and detect the reaction until 2-chlorofluorene is basically The response is complete. Stop chlorine flow, stir at 40°C for 2 hours, heat up and reflux until the reaction solution is completely dissolved and transparent, cool to room temperature, filter, the solid is 2,7-dichlorofluorene, ...

Embodiment 2

[0027] Example 2: Reductive dechlorination of 2,7-dichlorofluoreneacetic acid mother liquor zinc powder

[0028] Take 1 part of the mother liquor in Example 1, add it into a 250 mL four-necked bottle, add 13.1 g of zinc powder (0.2 mole) in batches at 20° C. under stirring, and complete the addition in about 30 minutes. Then react at 15°C for 2 h, filter, wash the solid with 10 ml of acetic acid, and combine the filtrates to become a colorless transparent liquid. Detected by liquid chromatography, the content of each relevant component is shown in Table 2.

[0029] Table 2, the ratio of each component of the mother liquor after zinc powder treatment

[0030]

Embodiment 3

[0031] Embodiment 3: the mother liquor of reductive dechlorination is chlorinated again

[0032] Add the mother liquor after reductive dechlorination in the above example 2 into a 250mL four-neck bottle, maintain the internal temperature at about 40°C and pass in chlorine gas while stirring, and track and detect the reaction by high performance liquid chromatography until the 2-chlorofluorene basically reacts completely. Stop the chlorine flow, stir at 40°C for 2h (the contents of the relevant components detected by liquid chromatography are shown in Table 3), first recover 50mL of acetic acid under reduced pressure below 60°C under the vacuum of the water pump, then heat up and reflux until the reaction solution is completely dissolved and transparent, and cool to After filtering at room temperature, the solid is 2,7-dichlorofluorene, 5.6 g after drying, and the liquid phase content is 98.0% (0.023 mol). Mother liquor is a yellow transparent liquid (the content of each releva...

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Abstract

The invention relates to a recovery processing method of a 2,7-dichlorofluorene reaction mother solution, in particular to a method for reusing waste liquid after treatment. Reductive dechlorination is carried out on the 2,7-dichlorofluorene reaction mother solution through zinc powder to obtain a mixed liquid mainly composed of 2-chlorofluorene and fluorine, the mixed liquid is filtered to removethe zinc powder and zinc acetate, and directed chloridized or chloridized with the raw material fluorine to prepare 2,7-dichlorofluorene. The recovery processing method of the 2,7-dichlorofluorene reaction mother solution is applied to the recycling of the 2,7-dichlorofluorene reaction mother solution, and has the advantages of simple operation, cheap treatment and the like.

Description

technical field [0001] The application relates to a method for recovering and treating the reaction mother liquor of 2,7-dichlorofluorene, in particular a method for reusing the reaction waste liquor after treatment. Background technique [0002] The compound drug artemether (artemether plus lumefantrine) is the first antimalarial drug in my country, and it is also an original Chinese drug that has been widely recognized internationally. It overcomes the shortcomings of high recurrence rate of artemether and slow effect of lumefantrine, achieves complementary advantages, maximizes strengths and avoids weaknesses, and thus is widely used in the prevention or treatment of potential multi-drug resistant malaria. [0003] 2,7-Dichlorofluorene is an important intermediate of benzfluorenol. At present, in industry, fluorene is used as raw material, glacial acetic acid is used as solvent, chlorine gas is passed through at 40°C for chlorination, and 2,7-dichlorofluorene is prepared ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C25/22
CPCC07C1/26C07C17/12C07C17/23C07C2603/18C07C25/22C07C13/567
Inventor 沈润溥陈卫中史久豪刘健常凯凯裘江英沈彩云盛国栋丰诚杰
Owner SHAOXING UNIVERSITY
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