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A technology of epichlorohydrin and chloropropene, applied in the direction of organic chemistry, which can solve the problems of explosion hazard and lower reaction conversion rate
Inactive Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology
However, under the action of the catalyst, a part of hydrogen peroxide decomposes ineffectively during the reaction, which not only red
Method used
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Embodiment 1
[0014] Add 3-chloropropene and catalyst to the reactor first, stir and heat up to the bubble point temperature, after about 44°C, then add hydrogen peroxide at a uniform speed for reaction, the feeding time is 0.5h, the total reaction time is 1h, the reaction heat in the reaction process is passed through the organic steam The condensate is carried away by reflux. Feed mass ratio, chloropropene: 50% hydrogen peroxide: catalyst is 1: 0.3: 0.11.
[0015] During the reaction process, the highest gas phase oxygen concentration is 4.4%, the conversion rate of allyl chloride is 41.6%, and the invalid decomposition rate of hydrogen peroxide is 1.4%.
Embodiment 2
[0017] Add 3-chloropropene and catalyst to the reactor first, stir and heat up to the bubble point temperature, after about 46°C, then add hydrogen peroxide at a uniform speed for reaction, the feeding time is 1h, the total reaction time is 1.5h, the reaction heat in the reaction process is passed through the organic steam The condensate is carried away by reflux. Feed mass ratio, chloropropene: 50% hydrogen peroxide: catalyst is 1: 0.3: 0.11.
[0018] During the reaction process, the highest gas phase oxygen concentration is 1.9%, the conversion rate of allyl chloride is 41.4%, and the invalid decomposition rate of hydrogen peroxide is 1.8%.
Embodiment 3
[0020] Add 3-chloropropene, catalyst and hydrogen peroxide together into the reactor at room temperature, stir and heat up to the bubble point temperature, about 44°C-46°C, and the reaction time is 1h. Feed mass ratio, chloropropene: 50% hydrogen peroxide: catalyst is 1: 0.3: 0.11.
[0021] During the reaction process, the highest gas phase oxygen concentration is 22.8%, the conversion rate of allyl chloride is 40.6%, and the invalid decomposition rate of hydrogen peroxide is 3.8%.
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Abstract
The invention relates to a method for producing epoxy chloropropane by a phase transfer method, which comprises the following steps of: adding 3-chloropropene serving as a raw material and a catalyst into a reactor, stirring, heating to the bubble point temperature of between 44 and 46 DEG C, adding hydrogen peroxide serving as an oxidant, and reacting at the bubble point temperature, wherein reaction heat in the reaction process is taken away through organic steam condensation and reflow; the catalyst is quaternary ammonium phosphotungstate; the reaction time is 1 hour; and the mass ratio of the 3-chloropropene to 50 percent hydrogen peroxide to the catalyst is 1:0.3:0.11. Other solvents are not added in the reaction; the hydrogen peroxide is added at the temperature of between 44 and 46 DEG C, so that the epoxidation reaction is further promoted, and the conversion rate of the epoxidation reaction is improved; meanwhile, the increase of organic steam partial pressure is facilitated, gaseous oxygen is diluted, and the blasting danger of a gaseous phase of the reactor is effectively reduced.
Description
technical field [0001] The invention relates to a production method of epichlorohydrin, in particular to a method for producing epichlorohydrin by a phase transfer method. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product with a wide range of uses. The traditional epichlorohydrin production process is mainly propylene high-temperature chlorination method and propylene acetate method, and there is a large amount of "three wastes" pollution control problems in the process of saponification sewage discharge. With the advancement of the sustainable development strategy, the green synthesis route of epichlorohydrin with industrial value has become the focus of research in the industry. The current research mainly focuses on the exploration of the direct epoxidation process route of allyl chloride, using titanium silicon molecular sieve or phosphorus Tungstate is used as a catalyst, and hydrogen peroxide is used ...
Claims
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