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Industrial synthesizing and purifying method of bis (4-nitrophenyl) carbonate

A purification method and carbonate technology are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of reducing production costs, low energy consumption, and simple process

Active Publication Date: 2012-11-07
TONGLING JINTAI CHEM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is no specific industrial synthesis and purification method for synthesizing bis(4-nitrobenzene) carbonate in China. The present invention provides a safe, reliable and stable industrial-grade synthesis and purification method. The finished bis(4-nitrobenzene) The carbonate content can reach over 99%, the chroma is below 20 black, and the product yield is 99%

Method used

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  • Industrial synthesizing and purifying method of bis (4-nitrophenyl) carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Add 500ml of dichloromethane, 56.3g of p-nitrophenol, 20ml of water, 1.5g of sodium sulfite, and 0.2ml of triethylamine into the 1L reactor 4, and stir for 30 minutes; weigh 21g of triphosgene and dissolve it in 60ml of dichloromethane, Be made into triphosgene---dichloromethane solution; In reactor 4, slowly drip 38ml concentration respectively and be 34% sodium hydroxide solution and prepared triphosgene---dichloromethane solution; Control reaction process temperature, Not exceeding 25°C, stirring until the pH value no longer drops and the synthesis is complete. Add tap water to the oil collection tank 5 to wash the materials in the oil collection tank; after standing for stratification, put the lower organic phase into the distillation kettle 7 to distill and remove the solvent; add 70°C dimethyl carbonate to the distilled solution to dissolve Solid-state bis(4-nitrobenzene)carbonate, make it reach supersaturated solution, and the solid separated by centrifuge 9 ente...

Embodiment 2

[0015] Add 25L dichloromethane, 2.8kg p-nitrophenol, 2L water, 15g sodium sulfite, 12ml triethylamine successively in 50L reactor 4, stir for 30 minutes; Then take by weighing 1.1kg triphosgene and dissolve in 3L dichloromethane, Make triphosgene---dichloromethane solution; Slowly add 2L concentration of 34% sodium hydroxide solution and prepared triphosgene---dichloromethane solution in the reactor 4 respectively; Whole process temperature control When the temperature exceeds 25°C, the pH value becomes stable after stirring for 2 hours, and the synthesis ends. Add tap water to the oil collection tank 5 to wash the materials in the oil collection tank; after standing for stratification, put the lower organic phase into the distillation kettle 7 to distill and remove the solvent; add 70°C dimethyl carbonate to the distilled solution to dissolve Solid bis(4-nitrobenzene)carbonate, make it reach supersaturated solution, and the solid obtained after separation by centrifuge 9 ente...

Embodiment 3

[0017] Add 1500L, 165kg p-nitrophenol, 120L water, 0.9kg sodium sulfite, 0.8L triethylamine successively in 3000L reactor 4, stir for 30 minutes, then weigh 1.1kg triphosgene and dissolve it in 3L dichloromethane to form Triphosgene --- dichloromethane solution; 3 Add 34% sodium hydroxide solution to the flow rate of 0.18 m 3 Add triphosgene---dichloromethane solution at the flow rate of / h; after stirring for 2 hours, the measured pH value is stable and no longer drops, and the stirring is stopped; tap water is added to the oil collection tank 5 to wash the materials in the oil collection tank; after standing for stratification, Put the lower organic phase into the distillation pot 7 to distill and remove the solvent; add 70°C dimethyl carbonate to the distilled solution to dissolve the solid bis(4-nitrobenzene)carbonate to make it a supersaturated solution, and centrifuge The solid separated by the machine 9 enters the oven 10 for drying to obtain a bis(4-nitrobenzene)carbo...

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Abstract

The invention discloses an industrial synthesizing and purifying method for safely, stably and reliably synthesizing high-purity bis (4-nitrophenyl) carbonate by a simple process with low energy consumption and low cost. The method comprises the following synthesizing steps: adding dichloromethane and p-nitrophenol serving as raw materials, sodium sulfite serving as an antioxidant, triethylamine sereving as a catalyst, and tap water into a reaction kettle (4) in proportion and stirring for 30min; adding a mixed solution of sodium hydroxide solution with concentration being 34% from a sodium hydroxide solution storage tank (1) and triphosgene- dichloromethane mixed solution from a triphosgene- dichloromethane solution tank (2) into the reaction kettle (4); keeping the temperature in the reaction kettle (4) not higher than 25%, reacting for 2h and then discharging the materials into an oil trap (5) from the reaction kettle (4); and carrying out water washing, distilling, crystallizing and cooling, separating and drying sequentially to finally obtain the high-purity bis (4-nitrophenyl) carbonate product.

Description

technical field [0001] The invention relates to an industrial synthesis and purification method of bis(4-nitrobenzene) carbonate. Background technique [0002] Bis(4-nitrobenzene)carbonate is solid at room temperature with high purity. It can be used as a carbonylation reagent to replace highly toxic phosgene to synthesize carbonate compounds, and has certain application prospects. [0003] At present, there is no specific industrial synthesis and purification method for synthesizing bis(4-nitrobenzene) carbonate in China. The present invention provides a safe, reliable and stable industrial-grade synthesis and purification method. The finished bis(4-nitrobenzene) The carbonate content can reach over 99%, the chroma is below 20 black, and the product yield is 99%. Contents of the invention [0004] The object of the present invention is to provide a method for synthesizing high-purity bis(4-nitrophenyl)carbonate with simple process, low energy consumption, low cost, safet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/43C07C201/12
Inventor 余海王桂珍于婷徐利林章山成
Owner TONGLING JINTAI CHEM INDAL
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