Method for catalytic synthesis of sodium tetrathionate with loaded iodine

A technology of sodium tetrasulfate and elemental iodine, applied in the field of preparation of sodium tetrasulfate, can solve the problems of many side reactions, pollution, low yield and the like, and achieve the effects of avoiding toxicity, high reaction efficiency and high catalytic activity

Inactive Publication Date: 2017-07-04
XUZHOU WANBANG JINQIAO PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem mainly solved by the present invention is to provide a method for catalytically synthesizing sodium tetrathionate by loading ...

Method used

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  • Method for catalytic synthesis of sodium tetrathionate with loaded iodine
  • Method for catalytic synthesis of sodium tetrathionate with loaded iodine

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Example 1 The preparation method of activated carbon supported elemental iodine

[0017] Weigh the activated carbon that has been dried to constant weight and add it to 2.5% ethanol solution of iodine, stir at room temperature, filter with suction, rinse with ethanol several times until neutral, dry at 70°C to constant weight, put it in a desiccator, and weigh it after cooling. Weight, calculate the load. i.e. iodine loading = (W 1 -W) / W 1 ×100%, where: W 1 is the mass (g) of activated carbon after loading, and W is the mass (g) of activated carbon before loading.

Embodiment 2

[0018] Embodiment 2 The preparation method of chitosan loaded elemental iodine

[0019] Weigh chitosan dried to constant weight and add 2.5% iodine ethanol solution, stir at room temperature, filter with suction, rinse with ethanol several times until neutral, dry at 70°C to constant weight, put in a desiccator, Cool and weigh and calculate the load. i.e. iodine loading = (W 1 -W) / W 1 ×100%, where: W 1 W is the mass (g) of chitosan after loading, and W is the mass (g) of chitosan before loading.

Embodiment 3

[0020] Example 3 Preparation method of silica gel loaded elemental iodine

[0021] Weigh 200-300 meshes of silica gel dried to constant weight and add it to 2.5% iodine ethanol solution, stir at room temperature, filter with suction, rinse with ethanol several times until neutral, dry at 70°C to constant weight, and put it in a desiccator , cooling and weighing, and calculating the load. i.e. iodine loading = (W 1 -W) / W 1 ×100%, where: W 1 is the mass (g) of silica gel after loading, and W is the mass (g) of silica gel before loading.

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Abstract

The invention discloses a method for catalytic synthesis of sodium tetrathionate with loaded iodine. The method comprises the following concrete steps: successively adding sodium thiosulfate, water, loaded iodine and an organic solvent into a reactor, carrying out a reaction at 0 to 40 DEG C for 4 to 36 h, after completion of the reaction, carrying out filtering, dissolving a filter cake in water, carrying out filtering, adding a filtrate into a cold organic solvent, and carrying out recrystallization, filtration and drying so as to obtain a product, i.e., sodium tetrathionate. The method provided by the invention has the following advantages: (1) the method has mild reaction conditions, high catalytic activity and high reaction efficiency; (2) the loaded iodine is an oxidant, so the problems of toxicity generated by iodine sublimation and after-treatment troubles are avoided; and (3) the sodium tetrathionate is unstable and is easy to generate by-products like S and SO2 in the process of a production process, and a loaded agent facilitates adsorption of the by-products, so the product prepared by using the method has high purity.

Description

technical field [0001] The invention relates to a preparation method of sodium tetrathionate, in particular to a method for catalytically synthesizing sodium tetrathionate by loading elemental iodine. Background technique [0002] Sodium tetrathionate, as a denaturant of recombinant protein, is widely used in the process of biomedicine. At present, the preparation method of sodium tetrathionate mainly uses iodine, hydrogen peroxide, sodium dichromate or arsenic trioxide as oxidant, and oxidizes thiosulfuric acid Sodium tetrathionate is prepared from sodium, a large amount of hydrogen peroxide as an oxidant will produce gas, which is not conducive to the amplification of sodium tetrathionate preparation, sodium dichromate or arsenic trioxide as an oxidant will easily lead to heavy metal residues, and iodine as an oxidant, the generated by-products Sodium iodide is easy to remove, but elemental iodine is easy to sublimate, has certain toxicity, is not environmentally friendly,...

Claims

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Application Information

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IPC IPC(8): C01B17/64B01J27/06B01J31/06
CPCC01B17/64B01J27/06B01J31/06C01P2002/82C01P2006/80
Inventor 文良柱赵丹黄晓梅崔杉朱亮
Owner XUZHOU WANBANG JINQIAO PHARMA
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