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Synthesis method of solid chelating agent piperazine-N, N-sodium bis-dithiocarbamate

A technology of sodium bis-dithiocarbamate and a synthesis method, applied in the directions of organic chemistry, organic chemistry, etc., can solve the problems of inconvenient transportation and storage of liquid products, difficult preparation of solid products, and unsatisfactory product yields, and avoid the problems of Problems in storage and transportation, shortening of dripping time, effect of less by-products

Pending Publication Date: 2021-11-30
江西鸿运环保科技有限公司
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  • Claims
  • Application Information

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Problems solved by technology

[0004] In the existing BPD-K synthesis process, there are still problems such as long reaction time, difficult control of by-products in the synthesis process, difficult preparation of solid products, inconvenient transportation and storage of liquid products obtained, and high production costs.
The only piperazine-N,N-bisdithiocarbamate sodium (hereinafter referred to as BPD-Na) synthetic technology, because of the complex raw materials used, the proportion is not accurate enough, the reaction process is not easy to control, the reaction time is long, and the product yield is not enough Ideal, the cost of production and use is higher than that of BPD-K, etc., and it is not accepted by the market

Method used

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  • Synthesis method of solid chelating agent piperazine-N, N-sodium bis-dithiocarbamate
  • Synthesis method of solid chelating agent piperazine-N, N-sodium bis-dithiocarbamate
  • Synthesis method of solid chelating agent piperazine-N, N-sodium bis-dithiocarbamate

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preparation example Construction

[0039] The synthesis method of a solid chelating agent piperazine-N, N-bistetiocarbamine provided by the present invention includes the following steps:

[0040] Step S1, the secondary amine negative ionization stage of piperazine:

[0041] Anhydrous piperazine, tetramethylolide is added to water, stirred, then dissolved, then add a sodium hydroxide solution to heating the reaction for a period of time to obtain a solution A;

[0042] Step S2, the secondary amine negative ion and the dioxide double nucleophilic reaction stage:

[0043] Diulfide is added dropwise to the solution A obtained in step S1, the temperature is maintained and reacted to give a solution of sodium piperazine-N, N-Di diimethylhydrine.

[0044] Step S3, the crystallization stage:

[0045] The piperazine-N, N-double diimethylmethoamate solution obtained in step S2, carried out, solid-liquid separation, washing, drying, pulverine-N, N-bis diiminogenate crystalline solid;

[0046] Step S4, the secondary crystalli...

Embodiment 1

[0059] 157.5 g of deionized water was added to 500 ml of four-mouth flasks equipped with a thermometer, dropping funnel, and 49.5 g of anhydrous piperazine, 0.32 g of tetramethylguanidine, stirred; stir for 15-20 minutes, stay After all piperazine dissolve, 112.5 g of 40% sodium hydroxide solution was added to the four flasks, and stirring was continued for 10 minutes; after using a water bath to lower the solution temperature to below 30 ° C, start dripping from the drip drain into the four flasks Add 89.1 g of carbon sulfide, the dropwise time is 10-15 minutes, the temperature of the dripping process is maintained below 30 ° C; the carbon disulfide is added, heated to heat the temperature to the solution temperature of 42 ° C, withdraw the water bath, continue to continue The reaction was stirred for 10 minutes. After the reaction is completed, the solution is reduced to room temperature to obtain a solid product, washed, separated, dried, and powdered to obtain a white crystall...

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Abstract

The invention provides a synthetic method of a solid chelating agent piperazine-N, N-sodium bis-dithiocarbamate. The method comprises a secondary amine anion ionization stage of piperazine, a secondary amine anion and carbon disulfide dual nucleophilic reaction stage, a crystallization stage and a secondary crystallization stage. The synthesis method disclosed by the invention has the advantages of few types of raw materials, few synthesis steps, short reaction time and easiness in reaction control, and the prepared solid product is high in purity and high in yield and is more beneficial to storage and transportation. The synthesis method provided by the invention is simple to operate, low in equipment requirement and low in production cost, and the prepared piperazine-N, N-sodium bis-dithiocarbamate solid product is good in stability, and has a shelf life of three years. The piperazine-N, N-sodium bis-dithiocarbamate solid product has a good removal effect on heavy metal ions, has a good harmless treatment effect on fly ash, and meets the national standard.

Description

Technical field [0001] The present invention relates to the field of organic synthesis applications, and more particularly to a synthesis method of a solid chelating agent piperazine-N, N-bistetinine sodium methyl sodium. Background technique [0002] As the amount of garbage incineration is increasing, the development of safety and effective fly ash chelating agents, improve the water soluble and stability of the chelating agent, optimize the synthetic process, reduce the cost, and promote the commodity of the new chelating agent. It is especially important. [0003] Piperazine-N, N-Di Dithiocarbamate (hereinafter referred to as BPD) is a heavy metal chelating agent, also known as heavy metal traps, capture, and the like. The molecular weight is moderate and has a reasonable molecular spatial structure, with good chelation capture efficiency and settlement performance. Such chelating agents can be used in a variety of garbage burning fly ash stabilization, industrial wastewater ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/21A62D3/33A62D101/08
CPCC07D295/21A62D3/33A62D2101/08C07B2200/13
Inventor 杨书逸杨飞陶庆文周英玖石磊明徐三善周梅阳
Owner 江西鸿运环保科技有限公司
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