Method for separating mixtures containing anthracene alkylation reaction products
A separation method, an alkylation technology, applied in the field of separation, can solve the problems that the separation technology of anthracene alkylation reaction product system has not been reported yet, and achieve the effect of reducing the difficulty of operation, improving the purity and the total yield
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[0043] In the present invention, the conditions and methods for the anthracene alkylation can be carried out in a conventional manner in the art. Usually, the preparation method of alkyl anthracene comprises: in the presence of a catalyst, a raw material liquid containing anthracene and an alkylation solvent is contacted with an alkylating agent to carry out an alkylation reaction. Wherein, the raw material of alkylation reaction is anthracene, and the alkylation solvent is the inert organic solvent that can dissolve anthracene, for example, can be C 6 -C 12 The paraffins or cycloalkanes of benzene can also be one-, two- or multiple-substituents of benzene, wherein, the substituents in the one-, two- or multiple-substituents of benzene are C 1 -C 4 One or more of the alkyl and halogen elements; more preferably, the alkylation solvent is a benzene substitute; most preferably, the alkylation solvent is 1,3,5-trimethylbenzene.
[0044] In the present invention, the substance t...
Embodiment 1
[0067] The liquid acid methanesulfonic acid is used as a catalyst for the alkylation reaction. In a 300ml stirred reactor, 46g of anthracene, 80ml of mesitylene, and 3ml of methanesulfonic acid were charged. After sealing the reaction kettle, start the stirring and temperature rise control program, the speed is set to 1000 rpm, and the temperature is 165°C. After the kettle temperature reached the set value, 2-methyl-2-butene was introduced into the kettle through a feed pump, the total amount of feed was 15.1 g, and the feed rate was 0.66 g / min. When the olefin feed was completed, the reaction conditions were kept constant, and the reaction was continued for 270 minutes before the reaction was terminated. Methanesulfonic acid was removed by sedimentation and separation, and a small amount of material in the kettle was taken out for chromatographic analysis. The same experimental conditions were carried out 5 times, and the materials were collected to provide raw materials f...
Embodiment 2
[0073] The alkylation reaction was carried out according to the method of Example 1, except that the method for separating the mixture of the alkylation reaction products included: the operating temperature of the atmospheric distillation system was 165° C., and the solvent trimethylbenzene was distilled off. Then raise the temperature of the atmospheric distillation device to 220° C., send the molten solid material into the melting crystallizer, and feed the cooling medium to start cooling and crystallization. The cooling rate was 1.0°C / h, the crystallization temperature was 197°C, the amount of anthracene added as seed crystal accounted for 1% by weight of the mass of the molten mixture, and the crystal growth time was controlled at 1.5h. After the crystallization process is over, the uncrystallized feed liquid is discharged and sent to the vacuum distillation system. Slowly heat up and sweat the crystals in the crystallizer, the temperature rise rate is 0.6°C / h, the sweatin...
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