Hypochlorite preparation method
A technology of hypochlorite and calcium hypochlorite, applied in the direction of hypochlorite, hypochlorous acid, products, etc., can solve the problems of easy light or thermal decomposition, pungent odor, unstable hypochlorous acid, etc. The effect of easy availability of raw materials, low calcium ion concentration and low cost of raw materials
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[0024] The purpose of this invention is to provide a kind of method for preparing hypochlorite comparatively conveniently. The raw materials used are easy to obtain, much more stable than hypochlorous acid, convenient for transportation and storage, friendly working environment, and less pungent odor. The by-products can be removed by filtering the reaction product, and the method is simple and convenient.
[0025] Taking lithium hypochlorite as an example, the concrete method for preparing hypochlorite in the present invention is as follows:
[0026] 1. Dissolve lithium hydroxide in water to prepare a solution or suspension. Lithium nitrate, lithium sulfate, lithium carbonate can also be selected.
[0027] 2. A cold water bath to maintain the temperature range of the reaction system at 0-25°C, preferably 5-15°C.
[0028] 3. Slowly add calcium hypochlorite into the lithium hydroxide solution, add dropwise oxalic acid solution or pass in carbon dioxide while stirring.
[00...
Embodiment 1
[0037] Get 42g of lithium hydroxide monohydrate and dissolve in 200g of water to prepare lithium hydroxide solution. Place the reacting round-bottom flask in a cold water bath, and maintain the temperature at 5-15°C, the maximum not exceeding 20°C. Slowly add 72 g of calcium hypochlorite solid to the lithium hydroxide solution, and simultaneously add dropwise 430 g of oxalic acid solution with a concentration of 10%. Calcium hypochlorite and oxalic acid were added at the same rate. After the addition is complete, continue to react for 30 to 60 minutes. The white solid formed by the reaction was filtered to obtain a pale yellow clear filtrate. Evaporate the filtrate in vacuum below 50°C until the crystals are precipitated, then place it below 5°C for cooling and crystallization, filter to obtain crystals, and continue vacuum evaporation and cooling crystallization of the mother liquor. This step was repeated until no crystals were precipitated from the mother liquor. The fi...
Embodiment 2
[0039] Get 128g lithium sulfate monohydrate and dissolve in 350g water to prepare lithium sulfate solution. Place the reacting round-bottom flask in a cold water bath, and maintain the temperature at 5-15°C, the maximum not exceeding 20°C. Slowly add 143g of calcium hypochlorite solid to the lithium sulfate solution, and simultaneously add dropwise 750g of oxalic acid solution with a concentration of 12%. Calcium hypochlorite and oxalic acid were added at the same rate. After the addition is complete, continue to react for 30 to 60 minutes. The white solid formed by the reaction was filtered to obtain a pale yellow clear filtrate. Evaporate the filtrate in vacuum below 50°C until the crystals are precipitated, then place it below 5°C for cooling and crystallization, filter to obtain crystals, and continue vacuum evaporation and cooling crystallization of the mother liquor. This step was repeated until no crystals were precipitated from the mother liquor. The filtered cryst...
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