Equipment for producing potassium chloride reverse flotation reagent using granular copper-nickel catalyst
By designing a production equipment for granular copper-nickel catalysts and employing a combination of upward-tilting and downward-pressing stirring paddles, the gas-liquid-solid three-phase reaction is enhanced, solving the problems of poor stability and low conversion rate of powdered catalysts. This enables the efficient production of dodecylmorpholine, improving production efficiency and product purity.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- QINGHAI SALT LAKE JINGCHENG CHEMICAL CO LTD
- Filing Date
- 2025-06-12
- Publication Date
- 2026-05-26
Smart Images

Figure CN224271123U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of salt lake chemical technology, specifically to an equipment and method for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst. Background Technology
[0002] Dodecylmorpholine has been industrialized and applied as a potassium chloride reverse flotation agent. Currently, the production method of dodecylmorpholine is: using dodecyl alcohol and morpholine in a one-step catalyst synthesis, with no by-products and a simple process. A production scale of 1,000 tons / year has been built. However, this method has certain drawbacks. The catalyst used in the current industrial production of dodecylmorpholine is a powdered copper-nickel supported catalyst. Copper and nickel are easy to fall off, and the catalyst has poor stability. After the reaction to synthesize dodecylmorpholine, the product and the catalyst are difficult to separate, leading to a number of problems: (1) it is difficult to recover the powdered catalyst; (2) the number of times the powdered catalyst can be reused and its efficiency is poor; (3) the hydrogen distributor and pipeline are blocked; the finished reagent (oily) contains powdered catalyst and the copper and nickel content is as high as 190 ppm and 100 ppm, respectively; (4) the finished reagent (oily) contains powdered catalyst and the copper and nickel content is as high as 190 ppm and 100 ppm, respectively. Although targeted measures have been taken, such as adding settling agents and extending the settling time in the storage tank, it is difficult to eliminate the problem at its root. This seriously affects the production efficiency of enterprises and causes pollution to downstream products and salt fields, resulting in adverse environmental impacts.
[0003] Granulating powdered copper-nickel catalysts for the production of dodecylmorpholine has been a research direction in recent years. However, the currently disclosed granular copper-nickel supported catalysts exhibit low conversion rates in the production of dodecylmorpholine, failing to meet enterprise requirements. Analysis revealed that the reasons are twofold: firstly, the existing production equipment and processes are unsuitable; secondly, the auxiliary materials added during the granulation process of the granular copper-nickel supported catalysts reduce catalyst activity. Summary of the Invention
[0004] To address the shortcomings of existing technologies, this invention proposes a device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst, thereby improving the conversion rate of the dodecylmorpholine synthesis reaction and increasing the reusability of the catalyst.
[0005] This utility model provides a device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst. Its structure is as follows: the connecting plate at the upper end of the reactor is connected to the flange by bolts, the motor is connected to the stirring shaft, the stirring shaft extends through the center of the flange into the reactor, the stirring shaft is connected to the upper stirring paddle, and the stirring shaft is connected to the stirring basket.
[0006] The upper stirring paddle is a downward-pressure type. When the reaction liquid reaches the height of the upper stirring paddle, the upper stirring paddle can achieve downward-pressure stirring of the reaction liquid, so that the reaction liquid and the particulate catalyst can be fully contacted.
[0007] The flange is also provided with pipe port A, pipe port B and pipe port C. The upper end of pipe port A is connected to two-port connecting pipe A through an adapter. The upper end of pipe port B is connected to the arc-shaped opening of two-port connecting pipe B through an adapter. The lower end of pipe port A is connected to a gas guide pipe. The gas guide pipe extends to the bottom of the mixing basket and the lower end is circular. Multiple gas guide holes are provided below the circular part of the lower end of the gas guide pipe.
[0008] The two-port connecting pipe A has an arc-shaped upper port for liquid inlet, which is connected to the morpholine dripping device, and a straight upper port for gas inlet, which is connected to the hydrogen supply pipe.
[0009] The gas outlet at the upper end of the two-port connecting pipe B is connected to a reflux device, and the straight port at the upper end is a liquid collection port. Connecting to a liquid collection container enables the recovery and recycling of morpholine.
[0010] A sealing gasket, made of asbestos rubber sheet, is also provided between the connecting plate and the flange.
[0011] The reactor is equipped with a constant temperature heating jacket.
[0012] The mixing basket is a single-layer structure with no top cover. It is reinforced with fixing strips on both the top and bottom. The central shaft hole of the mixing basket is circular. A lower mixing blade is located below the mixing shaft, between the mixing basket and the lower circular portion of the air guide pipe. The vertical portion of the air guide pipe passes through the edge of the mixing basket. The lower mixing blade is an upward-opening type.
[0013] The mixing basket has 3-5 layers, which are detachably connected. The top layer is covered, and a square shaft hole is set in the center. The lower part of the mixing shaft is set as a square column. The side wall opposite to the mixing basket is equipped with 3-5 sets of curved baffles, and the vertical part of the gas guide pipe is located in the gap of the curved baffles. The function of the curved baffles is to disrupt the laminar flow of the liquid, increase the turbulence effect, and improve the solid-liquid-gas mixing efficiency.
[0014] The mixing basket and cover are both made of stainless steel mesh, with the edges reinforced with stainless steel plates; or they are both made of stainless steel plates with holes punched in them.
[0015] The beneficial effects of this utility model are as follows: The equipment for producing dodecylmorpholine provided by this utility model is designed for the characteristics of granular catalysts. It adopts the form of a stirring basket and uses a hydrogen gas flow to introduce morpholine gas, so as to achieve full contact and reaction between hydrogen and morpholine gas and granular catalyst. It adopts a combination of upward stirring and downward stirring, and when the gas comes out, it can effectively send the gas to the bottom of the catalyst mesh, which is conducive to the gas, liquid and solid three-phase reaction. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of the present utility model;
[0017] Figure 2 These are schematic diagrams of the flange structure in embodiments 1 and 2 of this utility model;
[0018] Figure 3 This utility model Figure 1 AA view;
[0019] Figure 4 This is a bottom view of position B in Embodiment 1 of this utility model;
[0020] Figure 5 This is a schematic diagram of the structure of Embodiment 2 of the present invention;
[0021] Figure 6 This utility model Figure 5 AA view;
[0022] In the diagram: 1. Reactor, 2. Gas inlet pipe, 3. Stirring basket, 4. Stirring shaft, 5. Connecting plate, 6. Flange, 7. Pipe port A, 8. Two-port connecting pipe A, 9. Liquid inlet, 10. Gas inlet, 11. Motor, 12. Two-port connecting pipe B, 13. Gas outlet, 14. Liquid collection port, 15. Pipe port B, 16. Upper stirring paddle, 17. Side support, 18. Lower stirring paddle, 19. Pipe port C, 20. Gas inlet hole, 21. Fixing component, 22. Curved baffle, 23. Square shaft hole. Detailed Implementation
[0023] Example 1: A device for producing potassium chloride reverse flotation reagent using granular copper-nickel catalyst, the structure of which is as follows: the connecting plate (5) at the upper end of the reactor (1) is connected to the flange (6) by bolts, the motor (11) is connected to the stirring shaft (4), the stirring shaft (4) extends through the center of the flange (6) into the reactor (1), the stirring shaft (4) is connected to the upper stirring paddle (16), and the stirring shaft (4) is connected to the stirring basket (3).
[0024] The upper stirring paddle (16) is a downward-pressure stirring paddle. When the reaction liquid reaches the height of the upper stirring paddle (16), the upper stirring paddle (16) can achieve downward-pressure stirring of the reaction liquid, so that the reaction liquid and the particulate catalyst can be fully contacted.
[0025] The flange (6) is also provided with pipe port A (7), pipe port B (15) and pipe port C (19). The upper end of pipe port A (7) is connected to the two-port connecting pipe A (8) through an adapter. The upper end of pipe port B (15) is connected to the arc-shaped opening of the two-port connecting pipe B (12) through an adapter. The lower end of pipe port A (7) is connected to the air guide pipe (2). The air guide pipe (2) extends to the bottom of the mixing basket (3) and the lower end is circular. Multiple air guide holes are provided below the circular part of the lower end of the air guide pipe (2).
[0026] The two-port connecting pipe A (8) has an arc-shaped upper port for liquid inlet (9) which is connected to the morpholine dripping device, and a straight upper port for gas inlet (10) which is connected to the hydrogen supply pipe.
[0027] The gas outlet (13) at the upper end of the two-port connecting pipe B (12) is connected to a reflux device, and the straight port at the upper end is a liquid collection port (14). It is connected to a liquid collection container to realize the recovery and recycling of morpholine.
[0028] A sealing gasket, made of asbestos rubber sheet, is also provided between the connecting plate (5) and the flange (6).
[0029] The reactor (1) is equipped with a constant temperature heating jacket.
[0030] The mixing basket (3) is a single-layer structure made of stainless steel mesh, with no top cover. It is reinforced with fixing strips (21) on the edges and both the top and bottom surfaces. The central shaft hole of the mixing basket (3) is circular. A lower mixing paddle (18) is also provided below the mixing shaft (4). The lower mixing paddle (18) is located between the mixing basket (3) and the lower circular portion of the air guide pipe (2). The vertical portion of the air guide pipe (2) passes through the edge of the mixing basket (3). The lower mixing paddle (18) is an upward-flipping type.
[0031] Example 2: A device for producing potassium chloride reverse flotation reagent using granular copper-nickel catalyst, the structure of which is as follows: the connecting plate (5) at the upper end of the reactor (1) is connected to the flange (6) by bolts, the motor (11) is connected to the stirring shaft (4), the stirring shaft (4) extends through the center of the flange (6) into the reactor (1), the stirring shaft (4) is connected to the upper stirring paddle (16), and the stirring shaft (4) is connected to the stirring basket (3).
[0032] The upper stirring paddle (16) is a downward-pressure stirring paddle. When the reaction liquid reaches the height of the upper stirring paddle (16), the upper stirring paddle (16) can achieve downward-pressure stirring of the reaction liquid, so that the reaction liquid and the particulate catalyst can be fully contacted.
[0033] The flange (6) is also provided with pipe port A (7), pipe port B (15) and pipe port C (19). The upper end of pipe port A (7) is connected to the two-port connecting pipe A (8) through an adapter. The upper end of pipe port B (15) is connected to the arc-shaped opening of the two-port connecting pipe B (12) through an adapter. The lower end of pipe port A (7) is connected to the air guide pipe (2). The air guide pipe (2) extends to the bottom of the mixing basket (3) and the lower end is circular. Multiple air guide holes are provided below the circular part of the lower end of the air guide pipe (2).
[0034] The two-port connecting pipe A (8) has an arc-shaped upper port for liquid inlet (9) which is connected to the morpholine dripping device, and a straight upper port for gas inlet (10) which is connected to the hydrogen supply pipe.
[0035] The gas outlet (13) at the upper end of the two-port connecting pipe B (12) is connected to a reflux device, and the straight port at the upper end is a liquid collection port (14). It is connected to a liquid collection container to realize the recovery and recycling of morpholine.
[0036] A sealing gasket, made of asbestos rubber sheet, is also provided between the connecting plate (5) and the flange (6).
[0037] The reactor (1) is equipped with a constant temperature heating jacket.
[0038] The stirring basket (3) has 3-5 layers, which are detachably connected. The top layer is covered, and a square shaft hole (23) is set in the center. The lower part of the stirring shaft (4) is set as a square column. 3-5 sets of curved baffles (22) are set on the side wall opposite to the stirring basket (3). The vertical part of the gas guide pipe (2) is located in the gap of the curved baffles (22). The function of the curved baffles (22) is to disrupt the laminar flow of the liquid, increase the turbulence effect, and improve the solid-liquid-gas mixing efficiency.
[0039] The mixing basket and lid are both made of perforated stainless steel plates.
Claims
1. An apparatus for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst, characterized in that, Its structure is as follows: the connecting plate (5) at the upper end of the reactor (1) is connected to the flange (6) by bolts, the motor (11) is connected to the stirring shaft (4), the stirring shaft (4) extends through the center of the flange (6) into the reactor (1), the stirring shaft (4) is connected to the upper stirring paddle (16), and the stirring shaft (4) is connected to the stirring basket (3).
2. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 1, characterized in that, The upper stirring paddle (16) is a downward-pressing stirring paddle.
3. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 2, characterized in that, The flange (6) is also provided with pipe port A (7), pipe port B (15) and pipe port C (19). The upper end of pipe port A (7) is connected to the two-port connecting pipe A (8) through an adapter. The upper end of pipe port B (15) is connected to the arc-shaped opening of the two-port connecting pipe B (12) through an adapter. The lower end of pipe port A (7) is connected to the air guide pipe (2). The air guide pipe (2) extends to the bottom of the mixing basket (3) and the lower end is circular. Multiple air guide holes are provided below the circular part of the lower end of the air guide pipe (2).
4. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 3, characterized in that, The two-port connecting pipe A (8) has an arc-shaped upper port for liquid inlet (9) which is connected to the morpholine dripping device, and a straight upper port for gas inlet (10) which is connected to the hydrogen supply pipe.
5. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 4, characterized in that, The gas outlet (13) at the upper end of the two-port connecting pipe B (12) is connected to the reflux device, and the straight port at the upper end is the liquid collection port (14).
6. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 5, characterized in that, A sealing gasket, made of asbestos rubber sheet, is also provided between the connecting plate (5) and the flange (6).
7. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 6, characterized in that, The reactor (1) is equipped with a constant temperature heating jacket.
8. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 7, characterized in that, The stirring basket (3) is a single layer with no top cover. It is reinforced with fixing strips (21) on both the top and bottom. The central shaft hole of the stirring basket (3) is circular. A lower stirring paddle (18) is also provided below the stirring shaft (4). The lower stirring paddle (18) is located between the stirring basket (3) and the lower circular part of the air guide pipe (2). The vertical part of the air guide pipe (2) passes through the edge of the stirring basket (3). The lower stirring paddle (18) is an upward-turning stirring paddle.
9. The equipment for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 7, characterized in that, The stirring basket (3) is provided with 3-5 layers, which are detachably connected. The top layer is covered and a square shaft hole (23) is provided in the center. The lower part of the stirring shaft (4) is provided with a square column shape. 3-5 sets of curved baffles (22) are provided on the side wall opposite to the stirring basket (3). The vertical part of the air guide pipe (2) is located in the gap of the curved baffles (22).
10. An apparatus for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to any one of claims 8 or 9, characterized in that, The mixing basket and cover are both made of stainless steel mesh, with the edges reinforced with stainless steel plates; or they are both made of stainless steel plates with holes punched in them.