Method for producing high content diacetylene-benzene
A technology of diethynyl benzene and divinyl benzene, which is applied in the field of preparation of diethynyl benzene, can solve the problems of unsatisfactory purification results, difficulty in making time, increased equipment investment costs and operating costs, etc.
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[0018] The method for preparing diethynylbenzene (middle, right-mixed diethynylbenzene) of the present invention comprises the steps:
[0019] (1) Mix industrial-grade m-, p-mixed divinylbenzene (containing m-divinylbenzene, p-divinylbenzene, m-ethylstyrene, p-ethylstyrene and m-, p- Mixed diethylbenzene, among which, the content of p-mixed divinylbenzene is 80%) is dissolved in halogenated hydrocarbons (such as carbon tetrachloride, etc.), and then liquid bromine is added dropwise for reaction. The amount of liquid bromine It is: the ratio of its moles to the total moles of carbon-carbon double bonds in divinylbenzene=(1.05~1.2): 1, after the dropwise addition is completed, continue to stir for 1~3 hours, then heat up to reflux, so that the solid The materials are all dissolved, and then kept warm and cooled to 5-15°C. 1,4-bis-α, β-dibromoethylbenzene has low solubility in the above-mentioned solvents, so most of it is precipitated from the solution, filtered, and the mother...
Embodiment 1
[0025] (1) Bromination of divinylbenzene
[0026] In 200L carbon tetrachloride, add 80Kg technical grade divinylbenzene (Shandong Dongda Chemical Industry (Group) Company produces, wherein contains m-divinylbenzene 54.7%, p-divinylbenzene 25.2%, m, p -mixing ethyl styrene 20%), under the condition of avoiding light, slowly dropwise add 192Kg (1.2Kmol) liquid bromine while stirring, continue to stir for 1.5 hours after the dropwise addition is completed, at this moment, a large amount of white precipitates are formed, TLC shows After the reaction is complete, heat the material to reflux to dissolve all the solids, cool slowly to 5-15°C, and filter. The filtrate is a carbon tetrachloride solution rich in m-bis-α, β-dibromoethylbenzene, and is used for filter cakes. After washing with carbon tetrachloride and drying, 48 Kg (0.1 Kmol) of white solid (p-bis-α, β-dibromoethylbenzene, treated separately) was obtained, and the filtrate and washing liquid were combined.
[0027] (2) S...
Embodiment 2
[0031] (1) The bromination of divinylbenzene is the same as in Example 1.
[0032] (2) Synthesis of Diethynylbenzene
[0033] In 300L ethanol, slowly add 84Kg (1.5Kmol) potassium hydroxide under stirring, add 167Kg bromide after completely dissolving, control the temperature at 40-45°C, keep stirring for 1 hour, then add 84Kg (1.5Kmol) potassium hydroxide , then heated to reflux, and reacted for 0.5 hours. At this time, a large amount of white solids were formed. GC analysis showed that the reaction was complete. After the reaction, it was filtered, and the filter cake was potassium bromide. Diethynylbenzene was in the filtrate, which also contained excess of potassium hydroxide. Neutralize the filtrate with concentrated hydrochloric acid, a large amount of potassium chloride is generated at this time, filter to remove the salt. The filtrate is distilled off 2 / 3 ethanol under reduced pressure, and the residue is left standing, the diethynylbenzene is in the upper layer, and th...
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