Device for continuously oxidizing dimethyl sulfide by using reaction centrifuge
By employing a reaction centrifuge in the production of dimethyl sulfoxide (DMSO), utilizing baffles and two-phase weirs to separate the reactants, and combining this with a precooling heat exchanger and condenser, the problem of poor mass and heat transfer in traditional equipment was solved, enabling efficient, continuous production and high-yield DMSO preparation.
Patent Information
- Application Number
- CN202423040059.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-10
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2034-12-10
AI Technical Summary
Traditional dimethyl sulfoxide (DMSO) production equipment suffers from poor mass and heat transfer, slow reaction rate, long reaction time, poor separation effect, complex operation, low production continuity and throughput, and complex equipment.
The apparatus for the continuous oxidation of dimethyl sulfide using a reaction centrifuge includes a feeding device, a reaction centrifuge, and a discharging device. It utilizes baffles and two-phase weirs to separate the reaction mixture, and improves heat transfer efficiency through a cavity precooling heat exchanger. Combined with a condenser and a quality detection valve, it achieves efficient separation.
It improves mass transfer efficiency, shortens reaction time, simplifies operation, enables continuous production, improves product quality stability and yield, reduces power consumption, and reduces equipment footprint.
Smart Images
Figure CN223505298U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of chemical equipment, and particularly relates to a device for continuously oxidizing dimethyl sulfide by using a reaction centrifuge. BACKGROUND
[0002] Dimethyl sulfoxide (DMSO) is a kind of sulfur-containing organic compound with a molecular formula of C2H6OS, which is a colorless and odorless transparent liquid at room temperature and is a hygroscopic and flammable liquid. It has the characteristics of high polarity, high boiling point, good thermal stability, non-protic and water miscibility, and can be dissolved in ethanol, propanol, benzene and chloroform and most organic substances, and is known as "universal solvent". Dimethyl sulfoxide is generally prepared by dimethyl sulfide oxidation method. According to different oxidizing agents and oxidation methods, it usually includes nitric acid oxidation method, peroxide oxidation method, ozone oxidation method, anode oxidation method and nitrogen dioxide oxidation method.
[0003] The traditional process and production equipment have poor mass transfer, slow reaction rate and long reaction time. The separation effect is poor, and the operation is complex. The production continuity is poor, the processing capacity is small, and the equipment is complex. Therefore, it is urgent to have a new reaction method to solve the problems of mass transfer and heat transfer, improve the product yield, speed up the reaction speed, reduce the production cost and simplify the operation. SUMMARY
[0004] The application proposes a device for continuously oxidizing dimethyl sulfide by using a reaction centrifuge to solve the problems of low selectivity, long reaction time and non-continuous production caused by poor mass transfer and heat transfer of traditional equipment in the production process of dimethyl sulfoxide.
[0005] In order to achieve the above technical purpose, the application provides the following technical scheme: a device for continuously oxidizing dimethyl sulfide by using a reaction centrifuge, mainly comprising a feeding device, a reaction centrifuge and a discharging device, the feeding device, the reaction centrifuge and the discharging device are connected through a material pipeline;
[0006] The feeding device comprises a storage tank and a metering pump, the storage tank and the metering pump are connected through a material pipeline and are provided with a flow stop valve, the storage tank is a dimethyl sulfide storage tank and a hydrogen peroxide storage tank, and the metering pump is a dimethyl sulfide metering pump and a hydrogen peroxide metering pump;
[0007] The reaction centrifuge comprises a feeding port, a discharging port and a reaction centrifuge inner cavity; the feeding port comprises a light phase or mixed phase inlet and a heavy phase or mixed phase inlet, the discharging port comprises a light phase outlet and a heavy phase outlet, the light phase or mixed phase inlet and the light phase outlet are arranged on the same side of the reaction centrifuge, and the heavy phase or mixed phase inlet and the heavy phase outlet are arranged on the same side of the reaction centrifuge;
[0008] The reaction centrifuge is characterized in that: the lower part of the reaction centrifuge cavity is provided with a flow baffle, and the upper part is provided with two phase weirs, the two phase weirs are a light phase weir and a heavy phase adjustable weir respectively, the heavy phase adjustable weir is located at the upper part of the light phase weir; the flow baffle and the two phase weirs divide the reaction centrifuge cavity into a material mixing cavity, a reaction cavity, a light phase collection cavity and a heavy phase collection cavity, the heavy phase collection cavity is located at the upper part of the light phase collection cavity; a cavity pre-cooling heat exchanger is arranged outside the reaction centrifuge; the light phase outlet is connected with a condenser and then connected with a dimethyl sulfoxide water solution receiving tank, and the heavy phase outlet is connected with a dichloromethane receiving tank.
[0009] Further, the flow baffle is divided into a first flow baffle and a second flow baffle.
[0010] Further, the area of the first flow baffle is larger than that of the second flow baffle, and the first flow baffle is located at the lower part of the second flow baffle.
[0011] Further, the upper side of the light phase weir and the upper side of the heavy phase adjustable weir are both provided with a circular-arc convex flow slowing structure close to the outflow port.
[0012] Further, the cavity pre-cooling heat exchanger is provided with a heat exchange medium inlet and a heat exchange medium outlet.
[0013] Further, the internal medium of the cavity pre-cooling heat exchanger can be selected from any one of water, methanol, ethanol or ethylene glycol.
[0014] Further, the internal pipeline of the cavity pre-cooling heat exchanger is provided with flow slowing particles.
[0015] Further, the flow slowing particles are porous ceramic particles.
[0016] Further, the cavity pre-cooling heat exchanger is further provided with a temperature sensor.
[0017] Further, a material quality detection valve is arranged on the connecting pipeline between the condenser and the dimethyl sulfoxide water solution receiving tank.
[0018] The reaction centrifuge has the advantages that:
[0019] 1) The reaction centrifuge is adopted, so that the mass transfer efficiency is high, the raw materials are instantaneously fully mixed, the reaction rate is accelerated, and the reaction time is greatly shortened.
[0020] 2) The separation effect is good, the operation is simple, and the production efficiency is improved.
[0021] 3) The continuous production operation can be realized, the processing capacity is large, the power consumption is low, and the product quality stability is improved.
[0022] 4) high equipment integration, can reduce the floor space;
[0023] 5) high product yield, high purity. BRIEF DESCRIPTION OF DRAWINGS
[0024] Figure 1 For the utility model discloses a kind of continuous oxidation dimethyl sulfide devices using reaction centrifuge structure schematic view;
[0025] In the drawing,
[0026] 1-dimethyl sulfide storage tank, 11-dimethyl sulfide metering pump, 12-stop valve a;
[0027] 2-hydrogen peroxide storage tank, 21-hydrogen peroxide metering pump, 22-stop valve b;
[0028] 3-reaction centrifuge, 31-feeding port, 311-light phase or mixed phase inlet, 312-heavy phase or mixed phase inlet, 32-discharge port, 321-light phase outlet, 322-heavy phase outlet, 33-baffle, 331-first-stage baffle, 332-second-stage baffle, 34-reaction centrifuge inner cavity, 341-material mixing cavity, 342-reaction inner cavity, 343-light phase collection cavity, 344-heavy phase collection cavity, 35-light phase weir plate, 351-circular-arc protrusion flow-reducing structure a, 36-heavy phase adjustable weir plate, 361-circular-arc protrusion flow-reducing structure b, 37-driving servo motor, 371-transmission shaft, 38-cavity precooling heat exchanger, 381-heat exchange medium inlet, 382-heat exchange medium outlet, 383-temperature sensor, 39-turbine plate;
[0029] 4-condenser, 41-material quality detection valve;
[0030] 5-dimethyl sulfoxide aqueous solution receiving tank;
[0031] 6-dichloromethane receiving tank. DETAILED DESCRIPTION
[0032] In order to have more clear understanding on the technical features, objects and effects of the utility model, the specific implementation mode of the utility model will be explained by referring to the drawings.
[0033] As Figure 1 shown in one kind continuous oxidation dimethyl sulfide devices using reaction centrifuge, mainly including feeding device, reaction centrifuge 3, discharging device, feeding device, reaction centrifuge 3 and discharging device are connected through material pipeline;
[0034] The feeding device comprises a storage tank, a metering pump, a material pipeline connecting the storage tank and the metering pump and provided with a stop valve, the storage tank is a dimethyl sulfide storage tank 1 and a hydrogen peroxide storage tank 2, and the metering pump is a dimethyl sulfide metering pump 11 and a hydrogen peroxide metering pump 21; the dimethyl sulfide storage tank 1 and the dimethyl sulfide metering pump 11 are connected through a material pipeline and provided with a stop valve a12, and the hydrogen peroxide storage tank 2 and the hydrogen peroxide metering pump 21 are connected through a material pipeline and provided with a stop valve b22.
[0035] The reaction centrifuge comprises a feeding port 31, a discharging port 32 and a reaction centrifuge inner cavity 34; the feeding port 31 comprises a light phase or mixed phase inlet 311 and a heavy phase or mixed phase inlet 312, the discharging port 32 comprises a light phase outlet 321 and a heavy phase outlet 322, the light phase or mixed phase inlet 311 and the light phase outlet 321 are arranged on the left side of the reaction centrifuge 3, and the heavy phase or mixed phase inlet 312 and the heavy phase outlet 322 are arranged on the right side of the reaction centrifuge 3.
[0036] The lower part of the reaction centrifuge 3 inner cavity is provided with a flow baffle 33, and the upper part is provided with two phase weirs, the flow baffle 33 is divided into a first flow baffle 331 and a second flow baffle 332; the area of the first flow baffle 331 is greater than that of the second flow baffle 332, and the first flow baffle 331 is located below the second flow baffle 332; the two phase weirs are a light phase weir 35 and a heavy phase adjustable weir 36, and the heavy phase adjustable weir 36 is located above the light phase weir 35.
[0037] The upper side of the light phase weir 35 and the heavy phase adjustable weir 36 is provided with a circular-arc convex flow slowing structure, which is a circular-arc convex flow slowing structure a351 and a circular-arc convex flow slowing structure b361 respectively; the flow baffle 33 and the two phase weirs divide the reaction centrifuge inner cavity 34 into a material mixing cavity 341, a reaction inner cavity 342, a light phase collection cavity 343 and a heavy phase collection cavity 344, the heavy phase collection cavity 344 is located above the light phase collection cavity 343; the center position of the reaction centrifuge 3 inner cavity is a transmission shaft 371, the upper part of the transmission shaft 371 is connected with a servo motor 37, and the lower part is connected with a turbine plate 39.
[0038] The reaction centrifuge 3 is externally provided with a cavity pre-cooling heat exchanger 38; the cavity pre-cooling heat exchanger 38 is provided with a heat exchange medium inlet 381 and a heat exchange medium outlet 382; the internal medium of the cavity pre-cooling heat exchanger 38 can be selected from any one of water, methanol, ethanol or ethylene glycol.
[0039] The internal pipeline of the cavity pre-cooling heat exchanger 38 is provided with flow slowing particles; the flow slowing particles are porous ceramic particles; the cavity pre-cooling heat exchanger 38 is further provided with a temperature sensor 383, and the control temperature is 10-20℃.
[0040] The light phase outlet 321 is connected to the condenser 4, and then connected to the dimethyl sulfoxide aqueous solution receiving tank 5. A material quality detection valve 41 is arranged on the connecting pipeline between the condenser 4 and the dimethyl sulfoxide aqueous solution receiving tank 5. The heavy phase outlet 322 is connected to the dichloromethane receiving tank 6.
[0041] Example 2
[0042] The dimethyl sulfoxide collected by the device for continuously oxidizing dimethyl sulfide by using a reaction centrifuge is as follows:
[0043] 1) The dimethyl sulfide-containing dichloromethane solution and hydrogen peroxide are pumped into the inner cavity 34 of the reaction centrifuge by metering pumps, the molar ratio of dimethyl sulfide to dichloromethane is controlled to be 1:5, the reaction temperature is 0-10°C, the reaction residence time is 120s, the dimethyl sulfoxide aqueous solution is collected from the light phase outlet 321, and the dichloromethane is collected from the heavy phase outlet 322. The collected dimethyl sulfoxide aqueous solution and dichloromethane are analyzed by gas chromatography, and the conversion rate of dimethyl sulfide, the effective utilization rate of the oxidant, and the selectivity of dimethyl sulfoxide are calculated and listed in Table 1.
[0044] 2) The dimethyl sulfoxide is prepared by the same method as in Example 1, except that the molar ratio of dimethyl sulfide to dichloromethane is controlled to be 1:10. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of the oxidant, and the selectivity of dimethyl sulfoxide are listed in Table 1.
[0045] 3) The dimethyl sulfoxide is prepared by the same method as in Example 1, except that the molar ratio of dimethyl sulfide to dichloromethane is controlled to be 1:20. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of the oxidant, and the selectivity of dimethyl sulfoxide are listed in Table 1.
[0046] 4) The dimethyl sulfoxide is prepared by the same method as in Example 1, except that the molar ratio of dimethyl sulfide to dichloromethane is controlled to be 1:100. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of the oxidant, and the selectivity of dimethyl sulfoxide are listed in Table 1.
[0047] Table 1
[0048]
[0049] Example 3
[0050] The dimethyl sulfoxide collected by the device for continuously oxidizing dimethyl sulfide by using a reaction centrifuge is as follows:
[0051] 1) The dimethyl sulfide in dichloromethane solution, hydrogen peroxide were pumped into the inner cavity 34 of the reaction centrifuge by metering pump, the molar ratio of dimethyl sulfide: dichloromethane was controlled to be 1:20, the reaction temperature was 10-20℃, the reaction residence time was 120s, the dimethyl sulfoxide aqueous solution was collected from the light phase outlet 321; the dichloromethane was collected from the heavy phase outlet 322. The collected dimethyl sulfoxide aqueous solution, dichloromethane were analyzed by gas chromatography, and the conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfoxide were calculated. The results are listed in Table 2.
[0052] 2) The dimethyl sulfoxide was prepared by the same method as in Example 5, except that the reaction temperature was controlled to be 20-30℃. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfoxide are listed in Table 2.
[0053] 3) The dimethyl sulfoxide was prepared by the same method as in Example 5, except that the reaction temperature was controlled to be 30-40℃. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfoxide are listed in Table 2.
[0054] Table 2
[0055]
[0056] Example 4
[0057] The dimethyl sulfoxide was collected by the device for continuous oxidation of dimethyl sulfide using a reaction centrifuge, and the specific steps were as follows:
[0058] 1) The dimethyl sulfide in dichloromethane solution, hydrogen peroxide were pumped into the inner cavity 34 of the reaction centrifuge by metering pump, the molar ratio of dimethyl sulfide: dichloromethane was controlled to be 1:20, the reaction temperature was 20-30℃, the reaction residence time was 30s, the dimethyl sulfoxide aqueous solution was collected from the light phase outlet 321; the dichloromethane was collected from the heavy phase outlet 322.
[0059] The collected dimethyl sulfoxide aqueous solution, dichloromethane were analyzed by gas chromatography, and the conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfoxide were calculated. The results are listed in Table 3.
[0060] 2) The dimethyl sulfoxide was prepared by the same method as in Example 8, except that the reaction residence time was controlled to be 60s. The calculated conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfoxide are listed in Table 3.
[0061] 3) The same procedure as in Example 8 was used to produce dimethyl sulfoxide except that the reaction residence time was controlled to be 90 s. The calculated conversion of dimethyl sulfide, the effective utilization of oxidant, and the selectivity to dimethyl sulfoxide are listed in Table 3.
[0062] 4) The same procedure as in Example 5 was used to produce dimethyl sulfoxide except that the reaction residence time was controlled to be 150 s. The calculated conversion of dimethyl sulfide, the effective utilization of oxidant, and the selectivity to dimethyl sulfoxide are listed in Table 3.
[0063] Table 3
[0064]
[0065] The above examples are only the preferred technical solutions of the present application, and should not be regarded as a limitation of the present application. The protection scope of the present application should be the technical solutions recited in the claims, including the equivalent replacement solutions of the technical features recited in the claims, i.e. the equivalent replacement improvements within this range are also within the protection scope of the present application.
Claims
1. An apparatus for continuous oxidation of dimethyl sulfide with a reaction centrifuge, characterized by, Mainly including feeding device, reaction centrifuge, discharge device, feeding device, reaction centrifuge and discharge device are connected through material pipeline; The feeding device includes a storage tank and a metering pump, the storage tank and the metering pump are connected through a material pipeline and are provided with a flow stop valve, the storage tank is a dimethyl sulfide storage tank and a hydrogen peroxide storage tank, and the metering pump is a dimethyl sulfide metering pump and a hydrogen peroxide metering pump; The reaction centrifuge includes a feeding port, a discharging port and a reaction centrifuge cavity; the feeding port includes a light phase or mixed phase inlet and a heavy phase or mixed phase inlet, the discharging port includes a light phase outlet and a heavy phase outlet, the light phase or mixed phase inlet and the light phase outlet are arranged on the same side of the reaction centrifuge, and the heavy phase or mixed phase inlet and the heavy phase outlet are arranged on the same side of the reaction centrifuge; The lower part of the reaction centrifuge cavity is provided with a flow baffle, and the upper part is provided with two-phase weirs; the two-phase weirs are a light phase weir and a heavy phase adjustable weir, and the heavy phase adjustable weir is located above the light phase weir; the flow baffle and the two-phase weirs divide the reaction centrifuge cavity into a material mixing cavity, a reaction cavity, a light phase collection cavity and a heavy phase collection cavity; the heavy phase collection cavity is located above the light phase collection cavity; the center of the reaction centrifuge cavity is a transmission shaft, the upper part of the transmission shaft is connected with a servo motor, and the lower part is connected with a turbine plate; the outside of the reaction centrifuge is provided with a cavity precooling heat exchanger; the light phase outlet is connected with a condenser and then connected with a dimethyl sulfoxide aqueous solution receiving tank, and the heavy phase outlet is connected with a dichloromethane receiving tank.
2. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, The flow baffle is divided into a primary flow baffle and a secondary flow baffle.
3. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 2, wherein, The area of the primary flow baffle is greater than that of the secondary flow baffle, and the primary flow baffle is located below the secondary flow baffle.
4. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, Arc convex flow structure is arranged on the upper side of the light phase weir and the heavy phase adjustable weir near the outlet.
5. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, The cavity precooling heat exchanger is provided with a heat exchange medium inlet and a heat exchange medium outlet.
6. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 5, wherein, The internal medium of the cavity precooling heat exchanger can be selected from any one of water, methanol, ethanol or ethylene glycol.
7. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, The internal pipeline of the cavity precooling heat exchanger is provided with flow slowing particles.
8. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 7, wherein The flow slowing particles are porous ceramic particles.
9. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, The cavity precooling heat exchanger is also provided with a temperature sensor.
10. An apparatus for continuously oxidizing dimethyl sulfide using a reaction centrifuge as claimed in claim 1, wherein, A material quality detection valve is arranged on the connecting pipeline between the condenser and the dimethyl sulfoxide aqueous solution receiving tank.