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Method for preparing lithium hypochlorite through transformation of sodium hypochlorite

A technology of lithium hypochlorite and tert-butyl hypochlorite, applied in the directions of hypochlorous acid, hypochlorite, chemical instruments and methods, etc., can solve the requirements of increasing operation safety, increasing production cost, reducing yield, etc. problems, to avoid decomposition, improve effective chlorine, improve economic efficiency and safety effects

Pending Publication Date: 2021-03-26
GANFENG LITHIUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses highly toxic chlorine, which increases the requirements for operational safety, and the hypochlorite will decompose during distillation, which reduces the yield and increases production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 100.99g of tert-butanol to 1000g of available chlorine 9.5% hyposodium solution, start stirring, slowly add 152.62g of 32% hydrochloric acid dropwise, after the hydrochloric acid is added, let it stand for liquid separation, and obtain 172mL of tert-butyl hypochlorite solution, use 206.4 mL of pure water was stirred and washed for 20 minutes to obtain 157.4 mL (144.3 g) of tert-butyl hypochlorite. The tert-butyl hypochlorite was added to 314.8mL of pure water, then 55.86g of lithium hydroxide monohydrate was added to react until the upper organic phase became colorless, and the reaction was stopped, and the liquid separation was carried out to obtain a lithium hypochlorite solution. The lithium chlorate solution was put into a freeze dryer, freeze-dried for 2 days, and the temperature of the cold well was set at -60°C to obtain 29.2 g of white powdery solid lithium hypochlorite. The tested available chlorine content was 115.75%, and the Li content was 11.6%. The was...

Embodiment 2

[0035] Add 127.71g of tert-butanol to 1155g of 10.3% available chlorine hyposodium solution, start stirring, slowly add 191.12g of 32% hydrochloric acid dropwise, after the addition of hydrochloric acid, let it stand for liquid separation, and obtain 210.5mL of tert-butyl hypochlorite solution. Stir washing with 231.55 mL of pure water for 40 min to obtain 197.3 mL (180.79 g) of tert-butyl hypochlorite. The tert-butyl hypochlorite was added to 271.2 mL of pure water, then 69.98 g of lithium hydroxide monohydrate was added to react until the upper organic phase became colorless, and the reaction was stopped, and the liquid separation was carried out to obtain a lithium hypochlorite solution. The lithium chlorate solution was put into a freeze dryer, freeze-dried for 2 days, and the temperature of the cold well was set at -60°C to obtain 37.4 g of white powdery solid lithium hypochlorite. The tested available chlorine content was 105.67%, and the Li content was 10.44%. The waste...

Embodiment 3

[0037] Add 233.35g of tert-butanol to 2340g of 9.2% available chlorine hyposodium solution, start stirring, slowly add 345.85g of 32% hydrochloric acid dropwise, after the addition of hydrochloric acid, let it stand for liquid separation, and obtain 381.2mL of tert-butyl hypochlorite solution. Stir washing with 495.6 mL of pure water for 60 min to obtain 356.7 mL (328.2 g) of tert-butyl hypochlorite. The tert-butyl hypochlorite was added to 606.4 mL of pure water, then 127.05 g of lithium hydroxide monohydrate was added to react until the upper organic phase became colorless, and the reaction was stopped, and the liquid separation was carried out to obtain a lithium hypochlorite solution. The lithium chlorate solution was put into a freeze dryer, freeze-dried for 2 days, and the temperature of the cold well was set at -60°C to obtain 67.3 g of white powdery solid lithium hypochlorite. The tested available chlorine content was 112.95%, and the Li content was 11.17%. The waste l...

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PUM

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Abstract

The invention discloses a method for preparing lithium hypochlorite through transformation of sodium hypochlorite. The method for preparing lithium hypochlorite through transformation of sodium hypochlorite comprises the following steps: step A, slowly adding hydrochloric acid into a flask filled with tert-butyl alcohol and sodium hypochlorite, then standing for liquid separation, taking a lower-layer water phase as a sodium hypochlorite recovery liquid, and stirring and washing an upper-layer yellow oily matter with pure water once to obtain tert-butyl hypochlorite and a stirring and washingliquid; and B, adding tert-butyl hypochlorite obtained in the step A into pure water to react with a lithium source, stopping the reaction when an upper organic phase becomes colorless, and separatingliquid to obtain a lower water phase which is a lithium hypochlorite solution and an upper organic phase which is tert-butyl alcohol and can be directly recycled. According to the method for preparing lithium hypochlorite through transformation of sodium hypochlorite, cheap sodium hypochlorite is selected to replace conventional highly toxic gas chlorine to prepare lithium hypochlorite, and the economic benefits and safety of the method are improved. Lithium hypochlorite dehydration adopts freeze drying, decomposition of lithium hypochlorite is avoided, and available chlorine of the product is improved.

Description

technical field [0001] The invention relates to a method for preparing a high-efficiency disinfectant, in particular to a method for preparing high-purity lithium hypochlorite through sodium hypochlorite transformation. Background technique [0002] Lithium hypochlorite is commonly used in two types: solution and solid. The solution is light yellow, slightly chlorine-like, and poor in stability, while the solid is white powder. It is chemically stable below 40°C and easily soluble in water. It is a very Promising oxidants and disinfectants. High-purity lithium hypochlorite can also be used in polishing and etching of semiconductor materials. The common synthesis method of lithium hypochlorite is mostly reaction of chlorine gas and lithium hydroxide to produce a mixed solution containing lithium chloride and lithium hypochlorite, and the solution is purified and dehydrated to obtain lithium hypochlorite. [0003] Patent application number CN201810163330.0 discloses a prep...

Claims

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Application Information

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IPC IPC(8): C01B11/06
CPCC01B11/062
Inventor 李良彬廖萃胡志华潘志芳叶明曾飞强杨文君胡中胡斌曾宪勤
Owner GANFENG LITHIUM CO LTD
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