Bisoxalate preparation device and preparation method thereof

Abstract

The invention provides a bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device and method. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device comprises a feeding kettle, a diaphragm pump, a reaction kettle, a filter press, a distillation still and a vacuum pump. The feeding kettle, the diaphragm pump, the reaction kettle, the filter press, the distillation still and the vacuum pump are sequentially connected. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation method includes the following steps of inflation, feeding, pressurizing, mixing, reacting, heat preserving, discharging, and decompressing and drying. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device and method solve the technical problems that a bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation method in the prior art is slow in reaction and low in yield.

Description

Technical field [0001] The invention relates to the field of luminescent compound production, in particular to a bisoxalate preparation device and a preparation method thereof. Background technique [0002] As a new type of chemical cold light source, bis(2,4,5-trichlorosalicylic acid n-pentyl ester) oxalate is a kind of bisoxalate. It has high brightness and high efficiency chemiluminescent substance. Environmental protection, no electricity, safety and other features. [0003] There are two methods for preparing bisoxalate in the prior art. One process uses an equivalent amount of sodium metal or sodium hydride, resulting in high cost; after the reaction, a large amount of sodium chloride solid is generated, and the sodium chloride solid is washed with water. The product bis(2,4,5-trichlorosalicylic acid n-pentyl ester) oxalate is decomposed with water, resulting in low yield and poor product quality. [0004] The other process will produce a large amount of solid waste of trieth...

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Problems solved by technology

[0003] There are two methods for the preparation of bisoxalate in the prior art, one of which uses an equivalent amount of sodium metal or sodium hydride, resulting in a high cost; after the reaction, a large amount of sodium chloride solid is generated, and when the sodium chloride solid is washed with water, due to The product bis(2,4,5-trichlorosalicylate n-pentyl) oxalate is hydrolyzed resulting in low yield and poor product quality

[0004] Another process will produce a large amount of triethylamine hydrochloride or n-butylamine hydrochloride solid waste, which needs to be filtered out when separating the products, and triethylamine hydrochloride or n-butylamine hydrochloride are particularly easy to absorb moisture. Cause filtration and transfer to be very difficult, when reclaiming triethylamine or n-butylamine from triethylamine hydrochloride or n-butylamine hydrochloride, the water contained therein has a great impact on the reaction, and the yield is lower, that is, it cannot be applied mechanically. It is easy to realize; a large amount of triethylamine or n-butylamine is used as an acidic agent, which not only leads to high cost, but also is difficult to remove the moisture in triethylamine or n-butylamine, and the product bis(2,4, 5-n-pentyl trichlorosalicylate) oxalate is unstable, and decomposes when meeting water and alkali, so the reaction yield is very low, and the low yield causes the product to be refined, and the refining is very troublesome; the reaction time is also long

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