Micro-channel preparation method of tetra-n-butylammonium polyiodide

A technology of tetra-n-butylammonium and n-butylammonium, applied in chemical instruments and methods, preparation of amino compounds from amines, chemical/physical/physical-chemical processes, etc., can solve the problem of product decomposition, residual iodine, temperature sensitivity, etc. problem, to achieve the effect of good mass transfer effect, high yield and short reaction time

Inactive Publication Date: 2021-08-03
SHANGHAI INST OF TECH
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  • Abstract
  • Description
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Problems solved by technology

[0003] Because high polyiodine has both safe and efficient disinfection characteristics, strong basic quaternary ammonium salt anion exchange resin high polyiodine is used for disinfection of drinking water, but the residual iodine in the water after resin high polyiodine treatment is more, long-term drinking will also affect human health
Water-soluble polyiodine such as tetramethylammonium polyiodine and tetraethylammonium polyiodine are suitable for disinfection and sterilization in aquaculture, etc. The application of the aspect is very limited
Tetra-n-butylammonium iodide and iodine solution are often used to synthesize tetra-n-butylammonium polyiodine, but tetra-n-butylammonium polyiodine is sensitive to temperature, and traditional methods may cause product decomposition

Method used

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  • Micro-channel preparation method of tetra-n-butylammonium polyiodide
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  • Micro-channel preparation method of tetra-n-butylammonium polyiodide

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preparation example Construction

[0035] A kind of microchannel preparation method of tetra-n-butylammonium polyiodine, the method comprises the following steps:

[0036] (1) Tetra-n-butylammonium iodide ethanol solution and iodine ethanol solution are pumped into the microchannel reaction device respectively simultaneously, uniformly mixed and reacted to obtain a black flowing melt containing tetra-n-butylammonium high polyiodine; tetra-n-butylammonium In the butylammonium iodide ethanol solution, the concentration of the solute tetra-n-butylammonium iodide is 4-5mol / L; in the iodoethanol solution, the concentration of the solute iodine is 4-5mol / L;

[0037] (1-1) The tetra-n-butylammonium iodide ethanol solution in the first feed tank 1 and the iodine ethanol solution in the second feed tank 2 are pumped into the microstructure mixer 11 and mixed uniformly; The volume flow ratio of ammonium ethanol solution and iodine alcohol solution is (1-2): 1, preferably (1.5-2): 1;

[0038] (1-2) The mixed liquid is in...

Embodiment 1

[0042] The tetra-n-butylammonium iodide ethanol solution configured in the first feed tank 1, the tetra-n-butylammonium iodide ethanol solution, the proportioning of tetra-n-butylammonium iodide and ethanol is 1mol:200ml; In the second material The ethanol solution of iodine is configured in tank 2, and the proportioning of iodine and ethanol is 1mol:250ml. Wait to be pumped into the microstructure mixer 11 and enter the microchannel reactor 22 for reaction.

[0043] The first feed tank 1 and the second feed tank 2 are pumped into the microchannel reactor 22 according to the volume flow ratio, and kept at a certain temperature for a period of time, and the reaction solution from the microchannel reactor 22 is taken to detect four The productive rate and the purity of n-butylammonium polyiodine, specific conditions and results are shown in Table 1.

[0044] Embodiment 2-9 differs from Example 1 only in that the volume flow ratio of reaction temperature, retention time, tetra-n...

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Abstract

The invention relates to a micro-channel preparation method of tetra-n-butylammonium polyiodide, which comprises the following steps: (1) respectively and simultaneously pumping a tetra-n-butylammonium iodide solution and an iodine solution into a micro-channel reaction device, and uniformly conducting mixing and reacting to obtain a black flowing melt containing tetra-n-butylammonium polyiodide; and (2) cooling the melt to room temperature, condensing the melt into blocks, carrying out suction filtration, and conducting washing with ethanol to obtain the product tetra-n-butylammonium polyiodide. Compared with the prior art, the method has the advantages of simplicity, greenness, high energy utilization rate, low manufacturing cost, uniform heating and the like.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing a tetra-n-butylammonium polyiodine microchannel preparation method. Background technique [0002] Polyiodides are anionic compounds formed by the polymerization of iodide ions and multiple iodine molecules. High-polyiodine is not only widely used in conductive polymers and electrode materials, but also has important application value in the field of disinfection. It is a kind of safe and efficient disinfectant recognized by countries all over the world. Quaternary ammonium salt polyiodine is the most studied and applied type of polyiodine. Quaternary ammonium salt polyiodide is mainly used in the field of conductive materials, such as tetramethylammonium polyiodide, tetraethylammonium polyiodide, strong basic quaternary ammonium salt anion exchange resin polyiodine, etc. [0003] Because high polyiodine has both safe and efficient disinfection characteri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C211/63B01J19/00
CPCC07C209/68B01J19/0093C07C211/63
Inventor 邓维欧玉如徐正阳
Owner SHANGHAI INST OF TECH
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