Method for directly preparing iodine monochloride from iodine-containing salt

A technology of iodine monochloride and iodine salt, applied in the direction of interhalogen compounds, which can solve the problems of limited application range, increased transportation cost, high cost, etc., and achieve the effects of high product purity, reduced production cost, and improved reaction selectivity

Inactive Publication Date: 2019-12-17
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods (2) and (3) are simple to operate, the iodine monochloride generated cannot be extracted from the solution and can only be applied to some specific fields, which increases transportation costs and dangers
[0005] To sum up, the problems existing in the existing technical route are: using iodine as raw material to produce iodine monochloride, the cost is high and the domestic resource reserves and production capacity are insufficient and need to be imported. Once a trade dispute occurs or the price of raw materials rises, production will be affected.
Although the method for preparing iodine monochloride in a solution state is simple and convenient, the product is a solution that limits its scope of application and increases transportation costs.

Method used

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  • Method for directly preparing iodine monochloride from iodine-containing salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Put 50g of iodine-containing salt into a three-necked flask, fix it in an oil bath, connect the three-necked flask to a vacuum pump, turn on the vacuum pump to evacuate the three-necked flask to -0.1MPa, and heat the oil bath to 90°C , heat preservation and pressure holding for 4h, to obtain dry iodized salt;

[0023] (2) First lower the temperature of the oil bath to 40°C, then feed chlorine gas with a flow rate of 2g / h into the three-necked flask through the safety bottle, and maintain the pressure of the three-necked flask between 0.1MPa and 0.2MPa. The introduction of chlorine gas, potassium iodide gradually turns black, and changes from solid to liquid. When the amount of chlorine gas introduced reaches 70% of the stoichiometric amount, mechanical stirring is started. After the stoichiometric amount of chlorine gas is passed through, the stirring reaction is continued for 3 hours. After passing through the safety bottle and the concentrated sulfuric acid soluti...

Embodiment 2

[0028] (1) Add 1 kg of potassium iodide into the enamel reaction kettle and seal it, turn on the vacuum pump to evacuate the reaction kettle to -0.095MPa, turn on the heating mantle oil bath to heat the reaction kettle to 75°C, keep the temperature and pressure for 8 hours, and obtain dry potassium iodide ;

[0029] (2) First reduce the temperature of the reactor to 50°C, then feed chlorine gas with a flow rate of 50g / h into the reactor, and maintain the pressure of the reactor between 0.1MPa and 0.2MPa. When 75% of the stoichiometric amount, turn on the mechanical stirring. After the stoichiometric amount of chlorine gas is ventilated, continue to stir the reaction for 4h. After the reaction, the residual chlorine gas is passed into the NaOH aqueous solution with a mass fraction of 10%. The materials in the reaction kettle were transferred to an enamel filter and injected with nitrogen until the pressure was 0.1MPa-0.2MPa, and 735.4g of iodine monochloride was obtained by fil...

Embodiment 3

[0032] On the basis of embodiment 2, in embodiment 2 steps (1), 1kg potassium iodide is replaced into 5kg potassium iodide (its iodine content is 58.6wt% after analyzing) that reclaims from workshop, and pass into the chlorine gas in step (2) The flow rate was changed to 220g / h and the stirring reaction was continued for 6h after passing through the chlorine gas. Other conditions and steps were the same as in Example 2, and 3539.1g iodine monochloride was obtained by filtration.

[0033] The purity of the prepared iodine monochloride is 99.0wt% by titration with sodium thiosulfate standard solution, and the yield of iodine monochloride is 93.4% through weighing calculation.

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Abstract

The invention relates to a method for directly preparing iodine monochloride from iodine-containing salt, and belongs to the technical field of iodine monochloride preparation. According to the method, pure iodine monochloride is directly prepared through reaction of the iodine-containing salt and chlorine gas, generation of iodine trichloride is avoided mainly by controlling the chlorine gas introduction speed, the chlorine gas introduction amount and the reaction temperature, and the reaction selectivity is improved. The method disclosed by the invention is simple to operate and mild in reaction condition, the recovered iodine-containing salt is used as a raw material, the source of the raw material is widened, the cost of the raw material is reduced, the purity of the prepared iodine monochloride is 99 wt% or above, and the requirements of industrial production are met.

Description

technical field [0001] The invention relates to a method for directly preparing iodine monochloride from iodine-containing salt, and belongs to the technical field of preparation of iodine monochloride. Background technique [0002] Iodine monochloride is an important basic chemical raw material, which can be used as an iodination reagent, as an iodide on the benzene ring, and as a Webster's reagent (acetic acid or acetic acid-carbon tetrachloride solution of iodine monochloride) for Oil iodine value test. For example, triiodobenzene (diatrizoic acid) is the core functional group of the contrast agent, and the non-ionic monomeric contrast agents currently on the market such as iopamidol, iohexol, iopromide, ioversol, iotalamic acid Drugs such as and ioxilan are all derived and synthesized by intermediates generated by the following reaction equation. The synthesis method of the intermediate is prepared by reacting 3-aminoisophthalic acid derivatives with iodine monochlorid...

Claims

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Application Information

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IPC IPC(8): C01B7/24
CPCC01B7/24
Inventor 姚刚黄华璠张浩岳立平郑艺冀延治杨少飞振红
Owner PERIC SPECIAL GASES CO LTD
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