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A technology for the synthesis of hydroxylamine hydrochloride, which is applied in the fields of hydroxylamine, chemical instruments and methods, nitrogen compounds, etc., and can solve the problems of large amount of waste water, low yield, low purity, etc.
Active Publication Date: 2018-09-28
CHINA CATALYST HLDG CO LTD
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Problems solved by technology
To overcome the technical problems of large amount of waste water, long reaction cycle, low yield and low purity in the existing preparation method
Method used
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Embodiment 1
[0025] Put 100g (36.5%) hydrochloric acid and 141g pinacolone oxime into the reaction flask, raise the temperature to 70°C, react for 2 hours, cool and separate, and distill the water layer under reduced pressure. When solids precipitate in the flask, add 210g of ethanol to crystallize and filter to obtain Hydroxylamine hydrochloride, the results are shown in Table 1.
Embodiment 2
[0027] Put 100g (36.5%) hydrochloric acid and 141g pinacolone oxime into the reaction flask, raise the temperature to 75°C, react for 2 hours, cool and separate, and distill the water layer under reduced pressure. When solids precipitate in the flask, add 210g of ethanol to crystallize and filter to obtain Hydroxylamine hydrochloride, the results are shown in Table 1.
Embodiment 3
[0029] Put 100g (36.5%) hydrochloric acid and 141g pinacolone oxime into the reaction flask, raise the temperature to 70°C, react for 3 hours, cool and separate, and distill the water layer under reduced pressure. When solids precipitate in the flask, add 210g of ethanol to crystallize and filter to obtain Hydroxylamine hydrochloride, the results are shown in Table 1.
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Abstract
The invention discloses a hydroxylamine hydrochloride synthesis method which comprises the following steps: putting pinacolone oxime and a concentrated hydrochloric acid solution into a kettle in a mole ratio of 1.2-1.5 to 1, intensely stirring, heating to 70-80 DEG C, and carrying out hydrolysis; cooling, leaving to stand and layer, collecting an upper layer, namely pinacolone, and a lower layer,namely a hydroxylamine hydrochloride solution, carrying out vacuum distillation on a water layer, separating a white crystal in the kettle, adding ethanol, cooling, crystallizing, and filtering, so as to obtain hydroxylamine hydrochloride of high purity and high yield. By adopting the hydroxylamine hydrochloride synthesis method, side reactions in a hydrolysis process can be avoided, the purity of hydroxylamine hydrochloride can be improved, the yield of the hydroxylamine hydrochloride can be increased, in addition, the method has the characteristics of being simple in step, easy in raw material obtaining, small in wastewater amount, good in environmental-friendliness, and the like.
Description
Technical field [0001] The invention belongs to a method for synthesizing hydroxylamine salt, and relates to a method for synthesizing hydroxylamine hydrochloride. Background technique [0002] It is mainly used as a reducing agent and imaging agent, in organic synthesis for the preparation of oximes, and also as a raw material for the synthesis of anticancer drugs (hydroxyurea), sulfa drugs (sulfamethoxazole) and pesticides (metacarb). Used as a depolarizer in electroanalysis, as a short-term stop agent without coloring in the synthetic rubber industry, etc. The pharmaceutical industry is used as an intermediate of Trimoxazole. The synthetic dye industry is used for the preparation of isatin intermediates. Oil industry is used as antioxidant and antioxidant for fatty acid and soap. Analytical chemistry is used as a reducing agent for the analysis of formaldehyde, furfural, camphor and glucose. Depolarizer in electrochemical analysis. It is also used for the determination of...
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