Preparation of methyl ethyl ketazine by utilizing hydrogen peroxide method
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A hydrogen peroxide method, hydrogen peroxide technology, applied in the preparation of hydrazone, organic chemistry and other directions, can solve the problems of high cost investment and large potential safety hazards.
Inactive Publication Date: 2013-04-17
重庆蓝苗生物科技开发有限公司
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Problems solved by technology
However, 70% high-concentration hydrogen peroxide is used in the hydrogen peroxide method, which has great potential safety hazards. The production line must be equipped with a high-concentration hydrogen peroxide production line, and the initial cost investment is also high.
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Embodiment 1
[0019] Embodiment 1, raw material 1.45mol butanone 130ml, 1.49mol, the ammoniacal liquor 130ml of concentration 21.18%, the formamide 41ml of 0.97mol concentration 94%, inorganic oxide MO0.5g, disodium edetate 0.5g, concentration 25.76 % hydrogen peroxide 66g, 0.5mol, time, temperature and operating steps are as follows:
[0020] (1) Time 7:51, put methyl ethyl ketone, ammonia water, formamide, MO, and disodium ethylenediamine tetraacetate into the three-necked bottle in sequence, and the material temperature is 20°C. Start to add hydrogen peroxide (keep warm);
[0021] (2) The time is 8:45, the temperature is 40°C, and about 1 / 3 of the hydrogen peroxide is dripped in (to keep warm);
[0022] (3) The time is 9:40, the temperature is 44°C, and about 2 / 3 of the hydrogen peroxide is dripped;
[0023] (4) Time 10:44, temperature 44°C, hydrogen peroxide added (keep warm);
[0024] (5) Time 11:21, temperature 38°C, stop stirring, let stand, and separate layers;
[0025] 258.4 g o...
Embodiment 2
[0026] Example 2, butanone 129ml, ammonia water (27.87%) 105ml, formamide (89%) 40ml, MO0.5g, edetate disodium 0.5g, hydrogen peroxide (26.11%) 65.2g. The hydrogen peroxide was added dropwise at 23°C, and the drop was completed in 2 hours and 45 minutes, and the stirring was continued for 0.5 hours, and the yield was 88.72%.
Embodiment 3
[0027] Example 3, butanone 111ml, ammonia water (25.0%) 92ml, formamide (89%) 40ml. MO0.5g, disodium edetate 0.5g, hydrogen peroxide (26.11%) 65.2g. The process operation is the same as before, and the yield is 82.7%.
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Abstract
The invention discloses a formula and a production process for preparing methyl ethyl ketazine by utilizing a hydrogen peroxide method, which carries out an in-depth study on the hydrogen peroxide method, thereby improving the hydrogen peroxide method to form a ketazine production method suitable for the situations in China. In the method, hydrogen peroxide is used as an oxidant, ammonia and butanone (methyl ethyl ketone) are used as raw materials and formamide and an inorganic oxide are used as a catalyst and a cocatalyst respectively to interact with each other so as to prepare the ketazine, wherein the hydrogen peroxide belongs to an industrial product and has the concentration of 25% to 30%; ammonia is added in a form of ammonia water with the concentration of 20% to 25%; and the butanone, the formamide and the inorganic oxide are all in the industrial product level. The method disclosed by the invention can be used for solving the problems that the existing initial coarse products for producing hydrazine hydrate are low in concentration, high in energy consumption, low in efficiency and high in cost and the by-products are difficult to treat, thereby being suitable for the situations in China.
Description
technical field [0001] The invention relates to the field of chemical industry, and relates to a raw material for producing hydrazine hydrate, in particular to preparing butanoneazine by a hydrogen peroxide method. Background technique [0002] Ketazine is an intermediate for preparing hydrazine hydrate, and ketazine can be hydrolyzed to produce hydrazine hydrate. The preparation of ketazine plays an important role in the production process of hydrazine hydrate, and the preparation of ketazine is an indispensable step in the production of hydrazine hydrate by hydrogen peroxide method. [0003] Hydrazine hydrate is an important chemical product, which is widely used in pharmaceutical industry, agriculture, fine chemical industry and aerospace fields. There are many ways to prepare hydrazine hydrate, including the Raschig method of reacting sodium hypochlorite and ammonia, the urea method of reacting sodium hypochlorite and urea, and the ketazine method of adding aliphatic ke...
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