ChemicalBook CAS DataBase List Methanesulfonic anhydride

Methanesulfonic anhydride synthesis

13synthesis methods

Product Name:Methanesulfonic anhydride
CAS Number:7143-01-3
Molecular formula:C2H6O5S2
Molecular Weight:174.19

Methanesulfonic anhydride may be prepared by the dehydration of methanesulfonic acid with phosphorus pentoxide.
P2O5 + 6 CH3SO3H → 3 (CH3SO2)2O + 2 H3PO4
Methanesulfonic anhydride can be purified by distillation under vacuum (distillation of a solid) or by recrystallized from Methyl tert-butyl ether/toluene.

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75-75-2 Synthesis

75-75-2
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7143-01-3
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Yield:75-75-2 82%

Reaction Conditions:

with sulfuric acid;sulfur trioxide;dihydrogen peroxide at 50; under 75007.5 Torr;Large scale;

Steps:

1 process according to the invention with addition of water

In step A 352 kg of methane and 1923 kg of S03 are continuously fed to a reaction system consisting of 3 continuously stirred reactors. The solvent of the reaction is a mixture of sulfuric acid and the reaction product MSA. To minimize losses 498 kg/h sulfuric acid and 213 kg/h MSA are recycled from the bottom part of the distillation in step iv back to step i. As initiator 14kg/h of hydrogen peroxide (70 wt.-%, aqueous solution) are added, which is equivalent to about0.3 wt.-% H202 in the reaction mixture. The reaction system is operated under a methane pressure of 100 bar and at a temperature of 50 00. Under these conditions S03 conversion of 95 % is reached. In addition, hydrolysable by-products are formed. Stream i contains 21.3 wt.-% sulfuric acid, 69.9 wt.-% MSA, 3.2 wt.-%S03, 5 wt.-% of MSAA and 0.3 wt.-% CH4. The yield of MSA with regard to S03 is 82 % in stepIn step ii, 38 kg/h of water are added, while the system is still pressurized with 100 bar of methane. S03 and MSAA are converted to sulfuric acid and MSA, respectively.Then the reaction mixture is depressurized in step iii to ambient pressure. The compositions of the liquid and the gas phase in this step are summarized in Table 1.

References:

WO2020/212298,2020,A1 Location in patent:Page/Page column 10; 11

75-75-2 Synthesis

75-75-2
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7143-01-3
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$19.00/5g

References

96042-30-7 Synthesis