US 12,221,429 B2
Method for synthesizing 1,3,2-dioxathiolane 2,2-dioxide by in-situ catalytic oxidation
Qikui Liu, Shandong (CN); and Xiaomeng Zhang, Shandong (CN)
Assigned to Shandong Normal University, Jinan (CN)
Filed by Shandong Normal University, Shandong (CN)
Filed on Jul. 11, 2024, as Appl. No. 18/770,589.
Application 18/770,589 is a continuation of application No. PCT/CN2023/070353, filed on Jan. 4, 2023.
Claims priority of application No. 202211353140.8 (CN), filed on Nov. 1, 2022.
Prior Publication US 2024/0368111 A1, Nov. 7, 2024
Int. Cl. C07D 327/10 (2006.01); B01J 23/52 (2006.01); B01J 29/89 (2006.01); B01J 37/00 (2006.01); B01J 37/04 (2006.01); B01J 37/18 (2006.01)
CPC C07D 327/10 (2013.01) [B01J 23/52 (2013.01); B01J 29/89 (2013.01); B01J 37/0045 (2013.01); B01J 37/04 (2013.01); B01J 37/18 (2013.01)] 7 Claims
OG exemplary drawing
 
1. A method for synthesizing 1,3,2-dioxathiolane 2,2-dioxide (DTD) by in-situ catalytic oxidation, comprising the following steps:
(1) preparation of Au—Pd/titanium silicon (TS)-1 catalyst: dissolving a Pd salt and an Au salt in water, adding a TS-1 molecular sieve, followed by stirring uniformly, reacting for 8-24 h at a temperature raised to be 60-105° C., to obtain a reaction liquid, performing air-blast drying on the reaction liquid to remove the water to obtain white powder, and putting the obtained white powder into a tube furnace for reduction treatment at 350-450° C. for 2-3 h to obtain an Au—Pd/TS-1 catalyst, wherein the tube furnace has an atmosphere of a gas mixture of hydrogen and argon, the hydrogen in the gas mixture being at a volume concentration of 5-10%;
the Pd salt is one or two of PdCl2, PdSO4, Pd(NO3)2·2H2O or Pd(OAc)2;
the Au salt is AuCl3 and/or HAuCl4·3H2O; and
a mass ratio of the Pd salt, the Au salt, the TS-1 molecular sieve and the water is 8-12 g:8-15 g:0.9-1 kg:1-5 kg;
(2) preparation of raw materials: mixing the Au—Pd/TS-1 catalyst obtained in step (1) with water to obtain a suspension liquid at a mass concentration of 1-10%; and mixing glycol sulfite with dichloroethane to prepare a glycol sulfite-dichloroethane solution with a mass fraction of glycol sulfite of 10-60%, for later use; and
(3) continuous flow synthesis reaction: pumping the suspension liquid obtained in step (2) into a premixing zone of a flow reactor, introducing hydrogen and oxygen thereinto at the same time, and controlling a temperature of the premixing zone to be 10-90° C. and a residence time of the suspension liquid in the premixing zone to be 3-60 s, to obtain a premixed liquid, a volume ratio of the hydrogen to the oxygen being 1:1;
the premixed liquid entering a reaction zone after flowing out of the premixing zone, pumping the glycol sulfite-dichloroethane solution obtained in step (2) into the reaction zone at the same time, controlling a temperature of the reaction zone to be 10-90° C. and a residence time of a reaction to be 15-600 s, to obtain a reaction liquid, which flows out of the reactor, separating the Au—Pd/TS-1 catalyst by a filter, and processing an obtained filtrate by a centrifugal separator to obtain an aqueous phase and an organic phase; and
adding the same volume of deionized water to the organic phase, followed by pumping into a centrifugal extractor for liquid separation to obtain an organic phase solution, and distilling and crystallizing the obtained organic phase solution to obtain a DTD product.