Equipment and method for producing potassium chloride reverse flotation reagent by using granular copper-nickel catalyst

Abstract

The invention discloses equipment and a method for producing a potassium chloride reverse flotation reagent by adopting a granular copper-nickel catalyst, and relates to the technical field of salt lake chemical engineering. The equipment comprises a reaction kettle, a stirring shaft, a stirring paddle, a stirring basket, an upper stirring paddle, a lower stirring paddle and the like; on the basis of a powder catalyst, macroporous pseudo-boehmite and an acid solution are added, the powder catalyst is prepared into particles, and the particle type catalyst is matched with special production equipment to be used for producing the potassium chloride reverse flotation reagent. Compared with the prior art, the invention has the beneficial effects that the granular catalyst is combined with the special production equipment provided by the invention, the technical effect equivalent to the activity of a powder catalyst can be realized, the content of the target product is 85% or above, the highest content reaches 93.07%, the content of copper and nickel in the product is 10 ppm or below, the harm to salt pan brine is greatly reduced, and the production cost is reduced. The problem that flotation reagents and catalysts are difficult to separate which puzzles enterprises for many years is solved.

Description

Technical Field

[0001] The present invention relates to the technical field of salt lake chemical industry, in particular to a device and a method for producing a potassium chloride reverse flotation agent by using a granular copper-nickel catalyst. Background Art

[0002] Dodecylmorpholine has been industrialized and applied as a potassium chloride reverse flotation agent. At present, the production method of dodecylmorpholine is: catalytic synthesis of dodecanol and morpholine in a single step with a catalyst. There are no by-products and the process is simple. At present, a production scale of 1,000 tons / year has been established. However, this method has certain disadvantages. The catalyst used in the current industrial production of dodecylmorpholine is a powdered copper-nickel loaded catalyst. The 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, resulting in various problems: (1) the powder catalyst is difficult to recycle, (2) the powder catalyst is poor in the number of times and efficiency of reuse; (3) the hydrogen distributor and pipeline are blocked; the finished reagent (oily) is entrained with powder catalyst and the copper and nickel contents are as high as 190ppm and 100ppm; (4) the finished reagent (oily) is entrained with powder catalyst and the copper and nickel contents are as high as 190ppm and 100ppm. Although targeted measures have been taken, such as adding sedimentation aids, increasing the number of sedimentation tanks and extending the time, it is difficult to eliminate the problem fundamentally, which seriously affects the production efficiency of enterprises, pollutes downstream products and salt fields, and has adverse effects on the environment.

[0003] The use of powdered copper-nickel catalysts in the production of dodecylmorpholine after granulation has been a research focus in recent years. However, the currently available granular copper-nickel supported catalysts exhibit low conversion rates in the production of dodecylmorpholine, failing to meet industry requirements. Analysis revealed that this is due, in part, to the inadequacy of existing production equipment and processes, and in part, to the reduction in catalytic activity caused by the addition of auxiliary materials during the granulation process. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention proposes an apparatus and method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst. First, an auxiliary material more suitable for granulating the copper-nickel catalyst was developed. Furthermore, a dedicated apparatus for synthesizing dodecylmorpholine using the granular copper-nickel catalyst was developed. This improves the conversion rate of the dodecylmorpholine synthesis reaction and increases the catalyst's reusability.

[0005] The present invention provides an apparatus for producing a potassium chloride reverse flotation agent by using a granular copper-nickel catalyst. The apparatus comprises the following structure: a connecting plate at the upper end of a reactor is connected to a flange via bolts; a motor is connected to a stirring shaft; the stirring shaft passes through the center of the flange and extends into the reactor; the stirring shaft is connected to an upper stirring paddle and is connected to a stirring basket.

[0006] The upper stirring paddle is a downward pressure stirring paddle. When the reaction liquid reaches the height of the upper stirring paddle, the upper stirring paddle can realize downward pressure stirring of the reaction liquid, so that the reaction liquid is fully in contact with the granular catalyst.

[0007] The flange is also provided with pipe openings A, pipe openings B, and pipe openings C. The upper end of pipe opening A is connected to the two-port connecting pipe A through an adapter, and the upper end of pipe opening B is connected to the arc-shaped opening of the two-port connecting pipe B through an adapter; the lower end of pipe opening A is connected to the air guide pipe, which extends to the bottom of the mixing basket and has a circular lower end. A plurality of air guide holes are provided below the circular part of the lower end of the air guide pipe.

[0008] The two-port connecting tube A has an arc-shaped upper end as a liquid adding port connected to a morpholine adding device, and a straight upper end as a gas adding port connected to a hydrogen supply pipe.

[0009] The gas outlet at the upper end of the two-port connecting pipe B is connected to the reflux device, and the straight port at the upper end is a liquid collection port. It is connected to a liquid collection container to achieve the recovery and recycling of morpholine.

[0010] A sealing gasket is provided between the connecting plate and the flange plate and is made of asbestos rubber sheet.

[0011] The outside of the reactor is provided with a constant temperature heating jacket.

[0012] The mixing basket is single-layered, uncovered, and reinforced with fixing bars on both the top and bottom surfaces. The central axis hole in the mixing basket is circular, and a lower stirring paddle is located below the stirring shaft. The lower stirring paddle is located between the mixing basket and the circular portion at the lower end of the air guide tube. The vertical portion of the air guide tube passes through the edge of the mixing basket. The lower stirring paddle is an upward-turning stirring paddle.

[0013] The mixing basket is configured with three to five removably connected layers. The top layer has a cover and a centrally located square shaft hole. The lower portion of the mixing shaft is configured as a square column. Three to five sets of curved baffles are installed on the sidewalls opposite the mixing basket, with the vertical portion of the air duct located between the curved baffles. The curved baffles disrupt the laminar flow of the liquid, increase turbulence, and improve the efficiency of solid-liquid-gas mixing.

[0014] The mixing basket and cover are both made of stainless steel mesh, and the edges are reinforced with stainless steel plates; or both are made of stainless steel plates with holes; A method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst comprises the following steps: Step 1: prepare a granular catalyst. Weigh a certain amount of binder powder, add the prepared acid solution dropwise thereto, stir while adding, prepare it into a paste, let it stand for 4-8 hours, then add the powdered catalyst, mix it thoroughly with a kneader, extrude it into strips on an extruder, cut it into a length of 1-2 mm, and then program the temperature to dry and calcine it to 500°C, calcine it for 2 hours, and obtain a granular catalyst.

[0015] Table 1 Calcination temperature program of particle catalyst stage Heating section ℃ Heating time min Retention temperature ℃ Residence time min 1 20-100 30 100 2 2 100-200 30 200 2 3 200-300 30 300 2 4 300-400 30 400 2 5 400-500 60 500 120 Step 2: Weigh a certain amount of dodecanol and add it to the reactor. Place the prepared granular catalyst into a stirring basket and immerse it in the dodecanol. Slowly heat the constant temperature heating jacket and start stirring. At the same time, nitrogen is passed through the air duct to replace the air. The stirring speed is 100-300 r / min. After heating to 150°C, start to switch to hydrogen flow at a fixed hydrogen flow rate and continue heating. Step 3: After heating to 200 ° C and maintaining stability, hydrogen is passed for 2 hours, and then morpholine is added dropwise under the condition of continuous hydrogen passing. The morpholine addition rate is controlled. After the morpholine is added dropwise into the reactor, it is vaporized and enters the reaction system under the influence of the hydrogen flow. The temperature is maintained constant. After the addition of morpholine is completed, the hydrogen is continued to be stirred for 15 minutes; Step 4: Turn off heating, stirring and hydrogen, wait until the temperature drops to room temperature, open the device, take out the product, and perform gas chromatography analysis on its content.

[0016] The acid solution is a 15% nitric acid solution, and the amount added is 30% of the total feed weight.

[0017] The binder is macroporous pseudo-boehmite, and the mass ratio of macroporous pseudo-boehmite to powdered catalyst is 1:1 or 3:2.

[0018] The shape of the granular catalyst is round, hollow cylindrical, or clover-shaped; the particle size of the granular catalyst is 1 mm to 3 mm.

[0019] The ratio of dodecanol to granular catalyst is 13-15:50, and the molar ratio of dodecanol to morpholine is 1:1.1. The beneficial effects of the present invention are as follows: the equipment for producing dodecylmorpholine provided by the present invention is designed according to the characteristics of a granular catalyst, adopts a stirring basket, and uses a hydrogen flow to introduce morpholine gas, so that hydrogen and morpholine gas can fully contact and react with the granular catalyst; and a combination of upward stirring and downward stirring is adopted, so that when gas emerges, the gas can be effectively delivered to the bottom of the catalyst net, which is conducive to the gas-liquid-solid three-phase reaction.

[0020] The present invention is based on the powder catalyst, by adding macroporous pseudo-boehmite and acid solution, the powder catalyst is prepared into granules, the longitudinal strength is greater than 35MPa, the specific surface area reaches 150m 2 / g, with a breakage rate of less than 3%. The granular catalyst produced by this process, combined with the dedicated production equipment provided by the present invention, has good activity and stability, and can achieve technical results equivalent to those of powdered catalysts. The target product content is above 85%, with a maximum content of 93.07%. The product is dark red and transparent with minimal shedding. The copper / nickel content in the product is below 10 ppm, significantly reducing the risk to salt field brine and resolving the difficult separation of flotation agents and catalysts that has plagued companies for many years.

[0021] The method of the present invention is used to prepare a potassium chloride reverse flotation agent. Although a granulation process is added and the production cost of the catalyst is slightly increased, the catalyst prepared by the method has excellent stability and can be recycled 10-13 times, thereby greatly reducing the total amount of catalyst used and reducing the overall production cost. The method also solves the problem of blockage of a hydrogen distributor and a pipeline, greatly improves production efficiency, and can further reduce labor operating costs in the later stage. At the same time, the copper and nickel contents in the synthesized agent are both less than 10 ppm, which has obvious environmental benefits and is of great significance to the protection of salt fields and the sustainable development and utilization of salt lake resources. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic structural diagram of embodiment 1 of the present invention; Figure 2 Schematic diagram of the flange structure of embodiments 1 and 2 of the present invention; Figure 3 For the present invention Figure 1 AA view; Figure 4 A bottom view of position B of embodiment 1 of the present invention; Figure 5 This is a schematic structural diagram of Example 2 of the present invention; Figure 6 For the present invention Figure 5 AA view; In the figure: 1. Reactor, 2. Air guide pipe, 3. Stirring basket, 4. Stirring shaft, 5. Connecting plate, 6. Flange, 7. Pipe opening 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 opening B, 16. Upper stirring paddle, 17. Side support, 18. Lower stirring paddle, 19. Pipe opening C, 20. Air guide hole, 21. Fixing part, 22. Curved baffle, 23. Square shaft hole. DETAILED DESCRIPTION

[0023] Example 1, an apparatus for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst, having the following structure: a connecting plate (5) at the upper end of a reactor (1) is connected to a flange (6) via bolts, a motor (11) is connected to a stirring shaft (4), the stirring shaft (4) passes through the center of the flange (6) and extends into the reactor (1), the stirring shaft (4) is connected to an upper stirring paddle (16), and the stirring shaft (4) is connected to a 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 is fully in contact with the granular catalyst.

[0025] The flange (6) is further provided with a pipe opening A (7), a pipe opening B (15), and a pipe opening C (19). The upper end of the pipe opening A (7) is connected to the second-port connecting pipe A (8) through an adapter, and the upper end of the pipe opening B (15) is connected to the arc-shaped opening of the second-port connecting pipe B (12) through an adapter; the lower end of the pipe opening A (7) is connected to the air guide pipe (2), and the air guide pipe (2) extends to the bottom of the mixing basket (3) and has a circular lower end. A plurality of air guide holes are provided below the circular portion of the lower end of the air guide pipe (2).

[0026] The two-port connecting tube A (8) has an arc-shaped upper end serving as a liquid addition port (9) for connecting to a morpholine addition device, and a straight upper end serving as a gas addition port (10) for connecting to a 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). Connected to a liquid collection container, the morpholine can be recovered and recycled.

[0028] A sealing gasket is provided between the connecting plate (5) and the flange plate (6), and is made of an asbestos rubber sheet.

[0029] The reactor (1) is provided with a constant temperature heating jacket on the outside.

[0030] The mixing basket (3) is configured as a single layer and is made of stainless steel mesh. The top surface is uncovered, and the edges and upper and lower surfaces are reinforced with fixing strips (21). The central axis hole of the mixing basket (3) is circular, and a lower stirring paddle (18) is provided below the stirring shaft (4). The lower stirring paddle (18) is located between the mixing basket (3) and the circular portion at the lower end of the air guide tube (2). The vertical portion of the air guide tube (2) passes through the edge of the mixing basket (3). The lower stirring paddle (18) is an upward-turning stirring paddle.

[0031] Example 2, an apparatus for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst, having the following structure: a connecting plate (5) at the upper end of a reactor (1) is connected to a flange (6) via bolts, a motor (11) is connected to a stirring shaft (4), the stirring shaft (4) passes through the center of the flange (6) and extends into the reactor (1), the stirring shaft (4) is connected to an upper stirring paddle (16), and the stirring shaft (4) is connected to a 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 is fully in contact with the granular catalyst.

[0033] The flange (6) is further provided with a pipe opening A (7), a pipe opening B (15), and a pipe opening C (19). The upper end of the pipe opening A (7) is connected to the second-port connecting pipe A (8) through an adapter, and the upper end of the pipe opening B (15) is connected to the arc-shaped opening of the second-port connecting pipe B (12) through an adapter; the lower end of the pipe opening A (7) is connected to the air guide pipe (2), and the air guide pipe (2) extends to the bottom of the mixing basket (3) and has a circular lower end. A plurality of air guide holes are provided below the circular portion of the lower end of the air guide pipe (2).

[0034] The two-port connecting tube A (8) has an arc-shaped upper end serving as a liquid addition port (9) for connecting to a morpholine addition device, and a straight upper end serving as a gas addition port (10) for connecting to a 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). Connected to a liquid collection container, the morpholine can be recovered and recycled.

[0036] A sealing gasket is provided between the connecting plate (5) and the flange plate (6), and is made of an asbestos rubber sheet.

[0037] The reactor (1) is provided with a constant temperature heating jacket on the outside.

[0038] The stirring basket (3) is provided with 3-5 layers, the layers are detachably connected, the top layer is provided with a cover, a square shaft hole (23) is provided in the center, and the lower part of the stirring shaft (4) is provided in a square column shape; 3-5 sets of curved baffles (22) are provided on the side wall opposite to the stirring basket (3), and the vertical part of the air guide tube (2) is located in the gap between the curved baffles (22). The function of the curved baffles (22) is to disrupt the laminar flow of the liquid, increase the turbulent effect, and improve the solid-liquid-gas mixing efficiency.

[0039] The mixing basket and the cover are both made of stainless steel plates with holes punched in them.

[0040] Example 3. A method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst. The granular catalyst is prepared by weighing 400 g of macroporous pseudo-boehmite powder, to which 343 g of a prepared 15% nitric acid solution is added dropwise with stirring to form a paste. After the paste is allowed to stand for 4-8 hours, 400 g of the powdered catalyst is added. The mixture is thoroughly mixed in a kneader and extruded into strips on an extruder. The strips are cut into lengths of 1-2 mm, and then programmed to dry and calcined to 500° C., and then calcined at 500° C. for 2 hours to obtain a granular catalyst.

[0041] 600 g of dodecanol was weighed and added to the reactor (1) of Example 2. 150 g of the prepared granular catalyst was placed in a stirring basket (3) and immersed in the dodecanol. The constant temperature heating jacket was slowly heated and stirred. At the same time, nitrogen was introduced from the air guide tube (2) to replace the air. The stirring speed was 100 r / min. After heating to 150°C, hydrogen was introduced at a fixed hydrogen flow rate of 0.5 L / min, and heating was continued. After heating to 210°C and maintaining stability, hydrogen was passed for 2 hours, and then morpholine was added dropwise while continuing to pass hydrogen. The morpholine addition rate was controlled. After the morpholine was added dropwise into the reactor, it was vaporized and entered the reaction system under the influence of the hydrogen flow. The temperature was maintained constant. The morpholine was added dropwise for 2-3 hours. After the addition of morpholine was completed, stirring and passing hydrogen was continued for 15 minutes. Turn off heating, stirring and hydrogen, wait until the temperature drops to room temperature, open the device, take out the product, and perform gas chromatography analysis on the content. The target product content is 92.50%; the copper / nickel content in the product is less than 10 ppm.

[0042] Example 4. A method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst. A granular catalyst is prepared in a pilot test. 18 kg of macroporous pseudo-boehmite powder is weighed, to which 15 kg of a prepared 15% nitric acid solution is added. The mixture is kneaded in a kneader to form a paste. After standing for 4-8 hours, 12 kg of powdered catalyst is added and thoroughly mixed in a kneader. The paste is extruded into strips on an extruder, automatically cut to a length of about 2 mm, and then programmed to dry and calcined to 500°C. The mixture is then calcined at 500°C for 2 hours to obtain a granular catalyst.

[0043] 600 g of dodecanol was weighed and added to the reactor (1) of Example 1. 150 g of the prepared granular catalyst was placed in a stirring basket (3) and immersed in the dodecanol. The constant temperature heating jacket was slowly heated and stirred. At the same time, nitrogen was introduced from the air guide tube (2) to replace the air. The stirring speed was 300 r / min. After heating to 150°C, hydrogen was introduced at a fixed hydrogen flow rate of 0.5 L / min, and heating was continued. After heating to 210°C and maintaining stability, hydrogen was passed for 2 hours, and then morpholine was added dropwise while continuing to pass hydrogen. The morpholine addition rate was controlled. After the morpholine was added dropwise into the reactor, it was vaporized and entered the reaction system under the influence of the hydrogen flow. The temperature was maintained constant. The morpholine was added dropwise for 2-3 hours. After the addition of morpholine was completed, stirring and passing hydrogen was continued for 15 minutes. Turn off heating, stirring and hydrogen, wait until the temperature drops to room temperature, open the device, take out the product, and perform gas chromatography analysis on the content. The target product content is 90.30%; the copper / nickel content in the product is less than 10 ppm.

[0044] Stability Test 1: After removing the product from the reaction apparatus of Example 3, 600 g of dodecanol was added again, and the reaction process of Example 3 was repeated, resulting in a target product content of 91.42%; the copper / nickel content in the product was less than 10 ppm. The test was repeated 8 times, and the target product content was greater than 85%, and the copper / nickel content in the product was less than 10 ppm. After repeating the test for the 13th time, the target product content was greater than 80%, and the copper / nickel content in the product was less than 10 ppm.

[0045] Stability test 2: After taking out the product from the reaction device of Example 4, 600 g of dodecanol was added again, and the reaction process of Example 4 was repeated 8 times, each time replacing a layer of catalyst in the stirring basket (3). The target product content was obtained to be above 85%, and the copper / nickel content in the product was less than 10 ppm.

Claims

1. A device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst, characterized in that: The structure is as follows: a connecting plate (5) at the upper end of a reactor (1) is connected to a flange (6) by bolts; a motor (11) is connected to a stirring shaft (4); the stirring shaft (4) passes through the center of the flange (6) and extends into the reactor (1); the stirring shaft (4) is connected to an upper stirring paddle (16); and the stirring shaft (4) is connected to a stirring basket (3); the upper stirring paddle (16) is a downward pressure stirring paddle.

2. The device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 1, characterized in that: The flange (6) is further provided with a pipe opening A (7), a pipe opening B (15), and a pipe opening C (19). The upper end of the pipe opening A (7) is connected to the second-port connecting pipe A (8) through an adapter, and the upper end of the pipe opening B (15) is connected to the arc-shaped opening of the second-port connecting pipe B (12) through an adapter; the lower end of the pipe opening A (7) is connected to the air guide pipe (2), and the air guide pipe (2) extends to the bottom of the mixing basket (3) and has a circular lower end. A plurality of air guide holes are provided below the circular portion of the lower end of the air guide pipe (2).

3. The device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 2, characterized in that: The two-port connecting tube A (8) has an arc-shaped upper end serving as a liquid addition port (9) connected to a morpholine addition device, and a straight upper end serving as a gas addition port (10) connected to a hydrogen supply pipe; the two-port connecting tube B (12) has a gas discharge port (13) at its upper end connected to a reflux device, and a straight upper end serving as a liquid collection port (14).

4. The device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 3, characterized in that: The stirring basket (3) is configured as a single layer, with no cover on the top surface, and fixed bars (21) are provided on the upper and lower surfaces for reinforcement. The central axis hole of the stirring basket (3) is circular, and a lower stirring paddle (18) is provided below the stirring shaft (4). The lower stirring paddle (18) is located between the stirring basket (3) and the circular portion at the lower end of the air guide tube (2), and the vertical portion of the air guide tube (2) passes through the edge of the stirring basket (3); the lower stirring paddle (18) is an upward-turning stirring paddle.

5. The device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 3, characterized in that: The stirring basket (3) is provided with 3-5 layers, the layers are detachably connected, the top layer is provided with a cover, a square shaft hole (23) is provided in the center, and the lower part of the stirring shaft (4) is provided in a square column shape; 3-5 sets of curved baffles (22) are provided on the side wall opposite to the stirring basket (3), and the vertical part of the air guide tube (2) is located in the gap between the curved baffles (22).

6. The device for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to any one of claims 4 or 5, characterized in that: The mixing basket and the cover are both made of stainless steel mesh, and the edges are reinforced with stainless steel plates; or both are made of stainless steel plates with holes punched in them.

7. A method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst, characterized in that: The device according to any one of claims 1 to 6 comprises the following steps: Step 1: Prepare a granular catalyst by weighing a certain amount of binder powder, adding the prepared acid solution dropwise thereto while stirring, preparing a paste, leaving it for 4-8 hours, then adding the powdered catalyst, mixing it thoroughly in a kneader, extruding it into strips on an extruder, cutting it into a length of 1-2 mm, and then drying and calcining it at a programmed temperature to 500° C. for 2 hours to obtain a granular catalyst; Step 2: weigh a certain amount of dodecanol and add it to the reactor (1); put the prepared granular catalyst into the stirring basket (3), immerse it in the dodecanol, slowly heat it with a constant temperature heating jacket and start stirring; at the same time, nitrogen is passed through the air guide tube (2) to replace the air; the stirring speed is 100 r / min; after heating to 150°C, start to switch to hydrogen flow; the hydrogen flow rate is fixed and continue heating; Step 3: When heated to 200°C, morpholine is added dropwise while continuously passing hydrogen gas. The morpholine addition rate is controlled. After the morpholine is added dropwise into the reactor, it is vaporized and enters the reaction system under the influence of the hydrogen gas flow. The temperature is maintained constant. After the addition of morpholine is completed, the hydrogen gas is continued to be stirred for 15 minutes. Step 4: Turn off heating, stirring and hydrogen, wait until the temperature drops to room temperature, open the device, and take out the product for gas chromatography analysis.

8. The method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst according to claim 7, wherein: The acid solution is a 15% nitric acid solution, and the amount added is 30% of the total feed weight.

9. The method for producing a potassium chloride reverse flotation agent using a granular copper-nickel catalyst according to claim 8, characterized in that: The binder is macroporous pseudo-boehmite, and the mass ratio of macroporous pseudo-boehmite to powdered catalyst is 1:1 or 3:

2.

10. The method for producing potassium chloride reverse flotation reagent using a granular copper-nickel catalyst according to claim 9, characterized in that: The shape of the granular catalyst is round, hollow cylindrical, or clover-shaped; the particle size of the granular catalyst is 1 mm to 3 mm.

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