Method for preparing dibenzenesulfonimide by solvent-free grinding method

Abstract

The invention relates to a method for preparing dibenzenesulfonimide by a solvent-free grinding method. According to the method, firstly, benzsulfamide and pure benzene sulfonyl chloride are put into a ball mill to be ground, so that the benzsulfamide and the benzene sulfonyl chloride are sufficiently and uniformly mixed at room temperature; then, solid NaOH is fed into the ball mill in different batches; the grinding is continuously performed; the temperature of a reactant is maintained to be lower than 60 DEG C; after the reaction is completed, the reactant is moved out from the ball mill; the reactants are dissolved by organic solvents; filtering is performed for removing generated NaCl; filter liquid is obtained; finally, the filter liquid is subjected to concentration crystallization, filtering and drying; a product is obtained. In the whole reaction process, the solvent is not needed; the environment pollution is reduced; the production cost is reduced. The atom utilization rate of the whole preparation process is high; the atom economic green and environment-friendly ideal is met; the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of bisbenzenesulfonimide, in particular to a method for preparing bisbenzenesulfonimide by a solventless grinding method. Background technique [0002] Bisbenzenesulfonimide (BBI for short) is an important organic chemical nickel softener and anti-impurity agent. In the electroplating industry, it is used as the primary brightener instead of saccharin, which has the advantages of good leveling effect and less consumption than saccharin. In addition, in recent years, with the wide application of electrophilic fluorinating reagent - N-fluorobisbenzenesulfonimide in the fluorination of organic matter, as the main raw material for the preparation of N-fluorobisbenzenesulfonimide, BBI demand further increased. The methods of synthesizing BBI that have been reported in the literature mainly contain the following several kinds at present: [0003] Chemical Engineer, reported on page 59 of November 2009, reacted...

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Problems solved by technology

In this method, NaH and tetrahydrofuran are relatively expensive and not suitable for industrial production.

[0005] In the Chinese patent CN101671285A, a kind of benzenesulfonamide and benzenesulfonyl chloride are reported in the aqueous sodium hydroxide solution to prepare the method of bisbenzenesulfonimide, although the productive rate is higher in this method, but the maximum temperature required for the reaction reaches 100~ 105°C, benzenesulfonyl chloride is easily hydrolyzed when it meets water at high temperature

[0006] Chem. Eur. J., 2013, 19, 16910 reported benzenesulfonyl chloride and benzenesulfonamide, in the presence of Et3N and DMAP, the reaction in dichloromethane can prepare bisbenzenesulfonyl imide, but the reaction used Both Et3N and DMAP are relatively expensive and not suitable for industrial production of bisbenzenesulfonimide

[0007] In 2016, it was reported in WO2016009448A1 that using acetonitrile as a solvent, benzenesulfonyl chloride and more than twice the equivalent of benzenesulfonamide under the action of Et3N can produce bisbenzenesulfonimide. In this method, the amount of benzenesulfonamide is large, and acetonitrile and Et3N are relatively expensive, not suitable for industrial production

[0008] The above-mentioned method for preparing bis-benzenesulfonyl imide mostly uses more expensive alkali or solvent, although some use cheap NaOH as alkali, all will use water as solvent, causing benzenesulfonyl chloride to be hydrolyzed in the reaction process, and the reaction is completed A large amount of waste water is produced, causing environmental pollution

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