Method for synthesizing hydroxylamine salt
A technology of hydroxylamine salt and cyclohexanone oxime, which is applied in the field of preparation of hydroxylamine salt, can solve the problems of low yield of hydroxylamine product, unindustrialization and the like, and achieves the effect of improving atom utilization rate and improving atom utilization rate
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[0028] Example 1
[0029] (1) Synthesis of cyclohexanone oxime reaction process: Weigh 0.6g TS-1 molecular sieve and place it in the reactor, then weigh out 15ml (833.3mmol) of water, 6.4ml (61.6mmol) of cyclohexanone with a content of 99.5% and 25% 10ml of ammonia (NH 3 The molar weight is 133.6mmol, H 2 The molar amount of O is 379.2mmol) was added to the reactor; then, stirring and heating, the reaction solution was heated from room temperature to 70°C, and 30% hydrogen peroxide 8ml (H 2 O 2 Molar weight is 79.7mmol, H 2 After the molar amount of O is 351.6 mmol), the reaction is completed at normal pressure for 0.25 h. The reaction liquid and the solid TS-1 catalyst were separated by centrifugation. Using toluene as the extractant, the organic phase in the reaction solution was extracted and separated, and the content of cyclohexanone oxime in the organic phase was analyzed by gas chromatography. The yield of the intermediate cyclohexanone oxime was calculated quantitatively ...
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[0033] Examples 2~3
[0034] The operation steps and reaction conditions of the hydrolysis of cyclohexanone oxime to hydroxylamine in implementation 1 are the same, except that the inorganic acid added in the hydrolysis process is 2ml of concentrated sulfuric acid with a content of 95% (H + Molar weight is 71.3mmol, H 2 O molar amount is 10.2mmol), 65% concentrated nitric acid 5ml (H + Molar weight is 72.5mmol, H 2 The molar amount of O is 136.6 mmol), and the final aqueous raffinate phase is hydroxylamine sulfate mother liquor and hydroxylamine nitrate mother liquor. The organic phase was analyzed by gas chromatography, and the yield of hydroxylamine was quantitatively calculated. The experimental results are shown in Table 2.
[0035] Table 2 The influence of the types of inorganic acids on the hydrolysis of cyclohexanone oxime to hydroxylamine
[0036] Example
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[0037] Example 4
[0038] The operation steps and reaction conditions are the same as in Example 1, except that during the hydrolysis of cyclohexanone oxime to produce hydroxylamine, the amount of concentrated hydrochloric acid added is changed to 0.5ml (H + Molar weight is 5.9mmol, H 2 The molar amount of O is 21.3 mmol). The organic phase was analyzed by gas chromatography, and the yield of cyclohexanone oxime in the reaction process (1) and the yield of hydroxylamine in the reaction process (2) were quantitatively calculated. The experimental results are shown in Table 3.
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