A kind of preparation method of dimethyl sulfone
A technology of dimethyl sulfone and dimethyl sulfide, which is applied in the field of preparation of dimethyl sulfone, can solve the problems that the application research of dimethyl sulfone has not been carried out well, and achieves the improvement of effective utilization rate, prolongation of service life, The effect of increasing selectivity
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[0009] The present invention provides a method for preparing dimethyl sulfone. The method includes contacting a liquid mixture with a catalyst under oxidation reaction conditions, the liquid mixture containing dimethyl sulfide and at least one oxidant.
[0010] According to the method of the present invention, at least part of the catalyst is a modified titanium silicon molecular sieve, that is, the catalyst is a modified titanium silicon molecular sieve, or the catalyst is a titanium silicon molecular sieve and a modified titanium silicon molecular sieve.
[0011] The modified titanium silicon molecular sieve is obtained by contacting the titanium silicon molecular sieve with at least one acid.
[0012] The acid is a generalized acid, and may be one or more of inorganic acid, organic acid and acid salt. The organic acid may be carboxylic acid and / or sulfonic acid, such as C 1 -C 6 Aliphatic carboxylic acid, C 6 -C 12 Aromatic carboxylic acid, C 1 -C 6 Aliphatic sulfonic acid and C 6...
Embodiment 1
[0056] (1) Preparation of modified titanium silicon molecular sieve
[0057] The titanium silicon molecular sieve TS-1 was mixed with hydrochloric acid (aqueous solution with a mass concentration of 36% by weight), and the resulting mixture was stirred and reacted at 90°C for 5 hours. The temperature of the resulting reaction mixture was lowered to room temperature and then filtered, and the resulting solid The phase material was dried to constant weight at 120°C to obtain a modified titanium silicate molecular sieve. Among them, the titanium silicon molecular sieve TS-1 is made of SiO 2 In total, the molar ratio of titanium silicon molecular sieve to HCl is 1:0.2. After characterization, compared with the raw material titanium silicon molecular sieve, the UV-Vis spectrum of the modified titanium silicon molecular sieve obtained has a peak height of absorption peak between 240-300 nm reduced by 3.1%. The pore volume determined by the static nitrogen adsorption method Reduce by 1...
Embodiment 2
[0061] Dimethyl sulfone was prepared by the same method as in Example 1, except that in step (2), hydrochloric acid was not used, that is, the pH value of the mixture formed by dimethyl sulfide, oxidant and solvent was not adjusted. The pH of the mixture of methyl sulfide, oxidant and solvent is 6.8.
[0062] The liquid phase mixture obtained when the reaction proceeded to 0.5 hours, 2 hours and 20 hours was analyzed by gas chromatography, and the conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfone were calculated. The results are listed in Table 1.
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