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A technology of methylene disulfonate and methane disulfonic acid, which is applied in the direction of organic chemistry to achieve the effects of improving efficiency, reducing pollution and reducing costs
Active Publication Date: 2017-08-29
泰兴华盛精细化工有限公司
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[0011] Technical problem to be solved: the present invention provides an improved synthesis method of methylene disulfonate aimed at many limitations existing in the current methylene disulfonate synthesis method
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Embodiment 1
[0021] Add 176 g of methanedisulfonic acid and 30 g of paraformaldehyde into a 1 L reaction flask, and stir mechanically for 15 minutes. Then 120 g of anhydrous magnesium sulfate was added to the above system, the temperature was raised to 100° C., and the reaction was carried out at 100° C. for 5 hours. After the reaction, the system was cooled, and the solid was extracted with 200 mL×3 methylene chloride, the insoluble matter was removed by filtration, and the filtrate was spin-dried to obtain 120 g of white methylene disulfonate product, with a yield of 64%. 1 H NMR (CDCl 3 ,400M), 4.83(s,2H), 5.97(s,2H).
Embodiment 2
[0023] Add 176 g of methanedisulfonic acid and 33 g of paraformaldehyde into a 1L reaction flask, and stir mechanically for 15 minutes. Then 144 g of anhydrous magnesium sulfate was added to the above system, the temperature was raised to 80° C., and the reaction was carried out at 80° C. for 6 hours. After the reaction was completed, the system was cooled, and the solid was extracted with 200 mL×3 methylene chloride, the insoluble matter was removed by filtration, and the filtrate was spin-dried to obtain 143 g of white methylene disulfonate product, with a yield of 76%. 1 H NMR (CDCl 3 ,400M), 4.83(s,2H), 5.97(s,2H).
Embodiment 3
[0025] Add 176 g of methanedisulfonic acid and 45 g of paraformaldehyde into a 1 L reaction flask, and stir mechanically for 15 minutes. Then 240 g of anhydrous magnesium sulfate was added to the above system, the temperature was raised to 70° C., and the reaction was carried out at 70° C. for 8 hours. After the reaction, the system was cooled, and the solid was extracted with 200 mL×3 methylene chloride, the insoluble matter was removed by filtration, and the filtrate was spin-dried to obtain 96 g of white methylene disulfonate product, with a yield of 51%. 1 H NMR (CDCl 3 ,400M), 4.83(s,2H), 5.97(s,2H).
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Abstract
The invention provides a methylene methanedisulfonate synthesis method. The methylene methanedisulfonate synthesis method comprises the following preparation steps: adding methane-disulfonic acid and paraformaldehyde to a reaction vessel, stirring and mixing, then adding anhydrous magnesium sulfate, heating to 70-100 DEG C, carrying out isothermal reaction for 5-8 hours, cooling to room temperature, extracting solids by using dichloromethane, filtering to remove insoluble substances, and carrying out spin dry on a filtrate to obtain white methylene methanedisulfonate. The methylene methanedisulfonate synthesis method has the beneficial effects that a novel dehydrating agent is used, thereby causing reaction to be pure and environment-friendly; an organic solvent does not need to be added; the stirring of the system is easy; the reaction is complete, thereby improving the yield of the generated methylene methanedisulfonate; the reaction time is short; the aftertreatment is convenient; and the mass production can be realized simply and convenient.
Description
technical field [0001] The invention belongs to the field of organic synthetic chemistry, in particular to a method for synthesizing methylene disulfonate. Background technique [0002] Lithium-ion batteries are widely used in various electronic products due to their high energy density, environmental friendliness, and high capacity. With the rapid development of lithium-ion batteries in many energy storage fields, their requirements for energy density, high-temperature performance, and safety performance are also getting higher and higher. In order to improve the performance of lithium-ion batteries, current research focuses on the selection of new cathode materials for batteries, and progress has been made. However, the decomposition of the electrolyte under high temperature or high voltage conditions leads to a decrease in battery cycle life, which becomes a key factor limiting the improvement of battery performance. [0003] Methylene disulfonate (structural formula is...
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