Continuous reactor for gas-oil-water-solid heterogeneous system
By designing a continuous reactor for a gas-oil-water-solid multiphase system and utilizing components such as draft tubes and mixers, the problems of the dimethyl disulfide production unit being unable to achieve continuous production and low product yield were solved, thus achieving efficient dimethyl disulfide production.
Patent Information
- Application Number
- CN202422592081.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2034-10-25
AI Technical Summary
Existing dimethyl disulfide production equipment cannot achieve continuous production and has low product yields. In particular, the dimethyl sulfate process has the problems of intermittent production and low product yields.
A continuous reactor for a gas-oil-water-solid multiphase system is designed, comprising a cylinder, a settler, and a draft tube. The draft tube is provided to separate the interior of the reactor into a primary reaction zone and a secondary reaction zone. Components such as a mixer, a reflux pipe, and a cooler are used to promote the rapid removal and uniform mixing of the reaction materials, thereby improving the reaction driving force and equilibrium conversion rate.
The continuous process of dimethyl disulfide production has been realized, which significantly improves the product yield and solves the problems of large equipment investment and low yield in traditional processes.
Smart Images

Figure CN223337298U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of fine chemical industry, in particular to a gas-oil-water-solid multiphase system continuous reactor. Background Art
[0002] Dimethyl disulfide is an important chemical raw material used in industrial solvents, catalyst deactivators, pesticide intermediates, coking inhibitors, pre-curing agents, odor calibrants (flavorings), and fuel and lubricant additives. Currently, domestic dimethyl disulfide production capacity falls far short of market demand, leaving the market to be filled through imports.
[0003] There are two main routes for the synthesis of dimethyl disulfide: the methyl mercaptan process and the dimethyl sulfate process. The methyl mercaptan process offers continuous production, high production capacity, and excellent product quality, but it is also complex and requires significant equipment investment, approximately five times the cost of the dimethyl sulfate process. Currently, the dimethyl sulfate process remains the predominant dimethyl disulfide process in China. While this process is mature, offers high product quality, and requires minimal equipment investment, it operates intermittently and produces low yields, making it unable to fully meet current daily production needs.
[0004] In order to solve the above problems of dimethyl disulfide produced by the dimethyl sulfate method, we need to design and develop a continuous reactor that meets the requirements of the gas-oil-water-solid multiphase system based on the continuous production process of the dimethyl sulfate method. Utility Model Content
[0005] In order to solve the problem that the current dimethyl disulfide production device cannot achieve continuous production and has a low product yield, the utility model provides a gas-oil-water-solid multiphase system continuous reactor, comprising a cylinder and a settler, the settler is arranged at the bottom end of the cylinder, a methyl sulfide gas phase outlet is arranged at the top of the cylinder to discharge methyl sulfide gas, an oil phase outlet is arranged at the upper part of the cylinder to discharge crude dimethyl disulfide, a water phase outlet is arranged at the middle and upper part of the cylinder to discharge the reaction liquid, and a solid phase outlet is arranged at the bottom of the settler to discharge solid sodium sulfate; a guide tube is arranged inside the cylinder, and a plurality of communication holes are evenly distributed on the guide tube, the inner side of the guide tube is a main reaction zone, and the annular gap between the cylinder and the guide tube is a secondary reaction zone.
[0006] As a preferred solution, a mixer is provided at the bottom of the guide tube, and a reflux pipe is provided at the water phase outlet to connect with the mixer.
[0007] Furthermore, a cooler and a slurry pump are provided in the reflux pipe at the water phase outlet so that the water phase can be quickly cooled and circulated to fully participate in the reaction.
[0008] As a preferred solution, the inlet pipes of the cylinder include a sodium polysulfide inlet pipe and a dimethyl sulfate inlet pipe connected to the guide cylinder, and a premixer is provided outside the cylinder to connect the sodium polysulfide inlet pipe and the dimethyl sulfate inlet pipe.
[0009] As a preferred solution, a liquid level controller is provided on the cylinder to control the liquid level to be above the water phase outlet and below 80% of the liquid level.
[0010] Furthermore, a slurry discharge pipeline is provided at the solid phase outlet, and the liquid level controller is electrically connected to a control valve of the slurry discharge pipeline.
[0011] As a preferred solution, a temperature measuring device is provided on the side of the cylinder and electrically connected to the cooler to control the operating efficiency of the cooler.
[0012] The beneficial effects of the utility model are:
[0013] 1. This utility model separates the reactor into a primary reaction zone and a secondary reaction zone by providing a draft tube, enabling timely removal of the reaction products from the primary reaction zone from the reaction system, thereby improving the equilibrium conversion rate of the reaction. The reaction products, dimethyl disulfide, dimethyl sulfide, and sodium sulfate, are rapidly removed from the reaction system through different nozzles, promoting the reaction to move toward the product reaction, increasing the reaction driving force, and significantly improving the product yield.
[0014] 2. The utility model separates solid sodium sulfate by gravity settling, and the clarified reaction liquid flows out of the reactor through the nozzle, is cooled by an external cooler, and then returns to the reactor, and then enters the main reaction zone through the mixer nozzle. The unreacted substances continue to react in the main reaction zone, and the product yield is further improved. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In order to make the content of the present invention more clearly understood, the present invention is further described in detail below based on specific embodiments and in conjunction with the accompanying drawings, wherein
[0016] Figure 1 A schematic structural diagram of the present utility model.
[0017] The reference numerals in the accompanying drawings are:
[0018] 1. Cylinder; 11. Gas phase outlet; 12. Oil phase outlet; 13. Water phase outlet; 14. Slurry discharge pipe; 15. Sodium polysulfide inlet pipe; 16. Dimethyl sulfate inlet pipe; 17. Temperature measuring device; 18. Liquid level controller; 2. Premixer; 3. Draft tube; 4. Mixer; 5. Settler; 51. Solid phase outlet; 6. Cooler; 7. Slurry pump. DETAILED DESCRIPTION
[0019] To illustrate the features of the present invention, the present invention will be further described below with reference to the accompanying drawings and embodiments.
[0020] Example:
[0021] See also Figure 1The embodiment of the utility model provides a gas-oil-water-solid multiphase system continuous reactor, including a cylinder 1 and a settler 5. The settler 5 is arranged at the bottom end of the cylinder 1. A methyl sulfide gas phase outlet 11 is arranged on the top of the cylinder 1 to discharge methyl sulfide gas, an oil phase outlet 12 is arranged on the upper part of the cylinder 1 to discharge crude dimethyl disulfide, a water phase outlet 13 is arranged on the upper middle part of the cylinder 1 to discharge the reaction liquid, and a solid phase outlet 51 is arranged on the bottom of the settler 5 to discharge solid sodium sulfate; by quickly removing different reaction products, dimethyl disulfide, methyl sulfide, and sodium sulfate, from the reaction system through different pipe ports, the reaction is promoted to move towards the product reaction, the reaction driving force is increased, and the product yield is significantly improved. The inlet pipes of the cylinder 1 include a sodium polysulfide inlet pipe 15 and a dimethyl sulfate inlet pipe 16 connected to the guide cylinder 3, and a premixer 2 is provided outside the cylinder 1 to connect the sodium polysulfide inlet pipe 15 and the dimethyl sulfate inlet pipe 16. The sodium polysulfide solution and dimethyl sulfate in the premixer are pre-reacted according to the optimal reaction material ratio, the reaction driving force is large, and the reaction yield is promoted.
[0022] A guide tube 3 is arranged inside the cylinder 1, and a plurality of communication holes are evenly distributed on the guide tube 3. The inner side of the guide tube 3 is the main reaction zone, and the annular gap between the cylinder 1 and the guide tube 3 is the secondary reaction zone. By arranging the guide tube, the interior of the reactor is divided into the main reaction zone and the secondary reaction zone, so that the reaction products of the main reaction zone can be removed from the reaction system in time, further promoting the improvement of the reaction equilibrium conversion rate.
[0023] In addition, to further increase the utilization efficiency of materials, a mixer 4 is provided at the bottom of the draft tube 3, and a reflux pipe is provided at the aqueous phase outlet 13 to communicate with the mixer 4. By using the mixer and the nozzle for mixing, the materials are evenly mixed and the temperature is uniform, without overheating or supercooling, significantly reducing the side reaction of dimethyl sulfate hydrolysis under alkaline conditions and greatly improving the product yield.
[0024] The reflux pipe of the aqueous phase outlet 13 is provided with a cooler 6 and a slurry pump 7 to enable the aqueous phase to be rapidly cooled and circulated to fully participate in the reaction. This embodiment adopts an external cooler, a forced circulation of a large flow rate to cool the reaction liquid in the main reaction zone and a mixed temperature control method, which avoids the inevitable temperature unevenness of traditional jacket heat exchange, slow reaction speed in the supercooling zone, and alkaline thermal decomposition of dimethyl sulfate in the superheating zone, thereby promoting an increase in reaction yield.
[0025] This embodiment also incorporates several adaptability improvements to the device, further enhancing its adjustability and applicability. First, a liquid level controller 18 is provided on the cylinder 1 to control the liquid level to be above the aqueous phase outlet 13 and below the 80% liquid level. A slurry discharge pipe 14 is provided on the solid phase outlet 51, and the liquid level controller 18 is electrically connected to the control valve of the slurry discharge pipe 14. Furthermore, a temperature measuring device 17 is provided on the side of the cylinder 1 and electrically connected to the cooler 6 to control its operating efficiency. The aforementioned self-adjustment configuration significantly enhances the device's adaptability.
[0026] The above embodiments and accompanying drawings are intended only to illustrate the technical solutions of the present invention and are not intended to limit the present invention. The present invention has been described in detail with reference to preferred embodiments. Those skilled in the art should understand that any changes, modifications, additions, or substitutions made by those skilled in the art within the spirit of the present invention do not depart from the spirit of the present invention and are intended to fall within the scope of the claims of the present invention. Other related technical structures not fully disclosed in this utility model are prior art in the art.
Claims
1. A gas-oil-water-solid multiphase system continuous reactor, comprising a cylinder (1) and a settler (5), wherein the settler (5) is arranged at the bottom end of the cylinder (1), and is characterized in that: The top of the cylinder (1) is provided with a methyl sulfide gas phase outlet (11) for discharging methyl sulfide gas, the upper part of the cylinder (1) is provided with an oil phase outlet (12) for discharging dimethyl disulfide crude product, the middle upper part of the cylinder (1) is provided with a water phase outlet (13) for discharging the reaction liquid, and the bottom of the settler (5) is provided with a solid phase outlet (51) for discharging solid sodium sulfate; A guide tube (3) is provided inside the cylinder (1), and a plurality of communication holes are evenly distributed on the guide tube (3). The inner side of the guide tube (3) is a main reaction zone, and the annular gap between the cylinder (1) and the guide tube (3) is a secondary reaction zone.
2. The gas-oil-water-solid multiphase system continuous reactor according to claim 1, characterized in that: A mixer (4) is provided at the bottom of the guide tube (3), and a reflux pipe is provided at the water phase outlet (13) to communicate with the mixer (4).
3. The gas-oil-water-solid multiphase system continuous reactor according to claim 1, characterized in that: The reflux pipe of the water phase outlet (13) is provided with a cooler (6) and a slurry pump (7) so that the water phase can be quickly cooled and circulated to fully participate in the reaction.
4. The gas-oil-water-solid multiphase system continuous reactor according to claim 1, characterized in that: The inlet pipes of the cylinder (1) include a sodium polysulfide inlet pipe (15) and a dimethyl sulfate inlet pipe (16) connected to the draft tube (3), and a premixer (2) is provided outside the cylinder (1) to connect the sodium polysulfide inlet pipe (15) and the dimethyl sulfate inlet pipe (16).
5. The gas-oil-water-solid multiphase system continuous reactor according to claim 4, characterized in that: The cylinder (1) is provided with a liquid level controller (18) to control the liquid level to be above the water phase outlet (13) and below the 80% liquid level.
6. The gas-oil-water-solid multiphase system continuous reactor according to claim 5, characterized in that: The solid phase outlet (51) is provided with a slurry discharge pipeline (14), and the liquid level controller (18) is electrically connected to a control valve of the slurry discharge pipeline (14).
7. The gas-oil-water-solid multiphase system continuous reactor according to claim 1, characterized in that: A temperature measuring device (17) is provided on the side of the cylinder (1) and is electrically connected to the cooler (6) to control the operating efficiency of the cooler.