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A kind of purification method of triiodomethane

A triiodomethane and purification method technology, which is applied in the field of triiodomethane purification, can solve the problems of low content of finished products, many impurities, and unsatisfactory products, and achieve the effect of stable product quality

Active Publication Date: 2019-03-01
NANJING CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of the finished product is low and there are many impurities, which cannot meet the needs of medicine and biochemistry for high-purity triiodomethane

Method used

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  • A kind of purification method of triiodomethane
  • A kind of purification method of triiodomethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 100ml of acetone into 100ml of ethanol, stir and mix to obtain a compound solvent. Add 40g of triiodomethane into the compound solvent, stir until all the solids are dissolved, filter, concentrate under reduced pressure in a water bath at 34°C with a vacuum of -0.06Mpa, and concentrate until no liquid drips out. Pour the concentrated solution into a 500ml beaker, place it in an ice-water bath, the temperature of the ice-water bath is 5-7°C, crystallize until a large amount of crystals are precipitated, centrifuge to obtain a wet material, dry at 35°C for 1 hour, and vacuum degree is -0.09Mpa to obtain three 35g of methyl iodide pure product, the finished product purity is 99.91%, the specific test results are shown in Table 1.

Embodiment 2

[0029] Add 50ml of diethyl ether into 150ml of petroleum ether with a boiling range of 60-90°C, stir and mix to obtain a compound solvent. Add 25g of triiodomethane into the compound solvent, stir until all the solids are dissolved, filter, concentrate under reduced pressure in a water bath at 25°C, the vacuum degree of reduced pressure is -0.08Mpa, and concentrate until no liquid drips out. Pour the concentrated solution into a 500ml beaker, place it in an ice-water bath, the temperature of the ice-water bath is 4-6°C, crystallize until a large amount of crystals are precipitated, centrifuge to obtain the wet material, dry at 30°C for 1.5h, and the vacuum degree is -0.1Mpa to obtain Triiodomethane pure product 21g, the finished product purity is 99.93%, and concrete detection result is shown in Table 1.

Embodiment 3

[0031] Add 100ml of acetone to 200ml of water, stir and mix to obtain a compound solvent. Add 75g of triiodomethane into the compound solvent, stir until all the solids are dissolved, filter, concentrate under reduced pressure in a water bath at 20°C, the vacuum degree of reduced pressure is -0.1Mpa, and concentrate until no liquid drips out. Pour the concentrated solution into a 500ml beaker, place it in an ice-water bath, the temperature of the ice-water bath is 1-3°C, crystallize until a large amount of crystals are precipitated, centrifuge to obtain a wet material, dry at 40°C for 1.5h, and the vacuum degree is -0.08Mpa to obtain Triiodomethane pure product 68g, finished product purity is 99.92%, concrete test result is shown in Table 1.

[0032] Table 1 Comparison of test results

[0033]

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PUM

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Abstract

The invention discloses a method for purifying iodoform. The method is conducted in the dark and includes the following steps that a good solvent and a poor solvent for iodoform are evenly mixed; the prepared compound solvent is added into iodoform and stirred and dissolved at room temperature; the obtained mixed system is filtered at room temperature; the obtained filtrate is subjected to reduced pressure concentration; the obtained concentrated solution is cooled and crystallized; mother liquor is removed from the obtained crystallization solution, drying is conducted, and purified iodoform is obtained. Iodoform obtained through the method is stable in quality, the mass content is larger than 99.9%, the purification process is simple, safe, quick and efficient, the compound solvent in use can be recycled after treatment, the requirements for green chemical industry and environmental protection are met, and the method has prospects in industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical purification, and in particular relates to a method for purifying triiodomethane. Background technique [0002] Triiodomethane, also known as iodoform, sea iodoform, and yellow iodine, has a yellow shiny crystallization in appearance, easily soluble in benzene and acetone, soluble in alcohol, ether, and chloroform, and slightly soluble in water, glycerin, and petroleum ether. It can sublime and gradually decompose under the action of air and light. It is mainly used as preservative and disinfectant in medicine and biochemistry. [0003] The structural formula of triiodomethane is as follows: [0004] [0005] The existing production process of triiodomethane is as follows: use acetone and sodium iodide as raw materials, stir and add sodium hypochlorite at low temperature, control the reaction temperature until the system is not cloudy, stop adding sodium hypochlorite dropwise, then stand stil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/38C07C19/07
CPCC07C17/38C07C19/07
Inventor 沈悦费荣杰李清洁
Owner NANJING CHEM REAGENT
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