Reaction device for preparing zirconocene dichloride

Abstract

The utility model provides a reaction device for preparing zirconocene dichloride, which comprises a closed reactor arranged in a constant-temperature water bath box, and a raw material dripping device, a protective gas input device and a stirring device which are arranged on the closed reactor, a cooling sleeve communicated with the constant-temperature water bath box is arranged on the periphery of the protective gas input device, a pusher of the raw material dripping device is adjusted to control the input speed of the solid raw materials, the gas generation device is started, protective gas and reaction gas are input into the closed reactor, and input of the reaction raw materials can be controlled in a balanced mode; and meanwhile, the chemical reaction is continuously promoted in an environment atmosphere filled with protective gas, so that the reaction efficiency and the product yield are improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of reactor especially relates to a reaction unit based on be used for preparation dichloro zirconocene. BACKGROUND

[0002] Halogenated metallocene compound is used as olefin polymerization reaction, organic synthesis reaction and UV curing accelerator's catalyst useful material. On the other hand, as a medicine raw material such as cell proliferation inhibitor, electronic material such as semiconductor film agent. At present, the preparation of dichloro zirconocene usually utilizes zirconium tetrachloride and cyclopentadiene and diethylamine reaction obtains.

[0003] In the preparation of dichloro zirconocene, it needs to be carried out under the condition of air isolation and waterless. Moreover, diethylamine, one of the raw materials for preparing dichloro zirconocene, is an extremely volatile organic compound, which has strong irritancy and corrosivity. In an open environment, diethylamine will quickly evaporate into the air, which not only loses the reactant, but also may cause harm to the environment and the operator. Diethylamine vapor dispersed in the air can form an explosive mixture with oxygen, which has the risk of explosion.

[0004] Therefore, in order to ensure the safety of the reaction and better control the reaction conditions, diethylamine and zirconium tetrachloride, cyclopentadiene need to be placed in a closed container during the reaction process. At the same time, raw material feeding device and device for replacing the gas in the closed container are provided on the closed container. This will be more conducive to improving the safety of preparing dichloro zirconocene. SUMMARY

[0005] In order to solve the above problems, the utility model provides a reaction device for preparing dichloro zirconocene, which adopts the following technical scheme.

[0006] A reaction device for preparing dichloro zirconocene, comprising a closed reactor arranged in a constant temperature water bath box, the closed reactor is provided with a stirring device and a plurality of interfaces, the closed reactor is provided with a solid raw material feeder, two liquid raw material drop feeders and a protective gas inputter,

[0007] The solid raw material feeder comprises a raw material pipe, a feeding pipe and a constant pressure pipe, the upper end of the raw material pipe is configured as a feeding hopper with a plug, the lower end of the raw material pipe is communicated with the transversely arranged feeding pipe, one end of the feeding pipe is communicated with the lower end of the constant pressure pipe, the upper end of the constant pressure pipe is communicated with the upper part of the raw material pipe, and the lower end of the constant pressure pipe is provided with a downward unsealed discharge port for sealed connection with the interface of the closed reactor;

[0008] The other end of the feeding pipe is provided with a rotating handle, the rotating handle is pivotally connected with a spiral auger in the feeding pipe, and the feeding pipe is rotationally connected with the spiral auger;

[0009] The liquid raw material dropper comprises a tube layer and a shell layer sleeved on the outer wall of the tube layer, a cavity filled with flowing cooling medium is formed between the tube layer and the shell layer, the upper end of the tube layer extending out of the shell layer is configured as a feeding hopper with a plug, a plug valve is arranged at the middle part of the lower end of the tube layer extending out of the shell layer, a joint of the tube layer below the plug valve is used for sealingly connecting with an interface of the closed reactor, one end of a balance pipe penetrates through the shell layer and communicates with the side wall of the tube layer, and the other end of the balance pipe communicates with the side wall of the joint below the plug valve.

[0010] The interface communicating with the solid raw material feeder and the liquid raw material dropper and the interface communicating with the protective gas inputter are both arranged on the upper end surface of the closed reactor.

[0011] The protective gas inputter comprises an inner pipe and an outer pipe sleeved on the outer wall of the inner pipe, a cavity filled with flowing cooling medium is formed between the inner pipe and the outer pipe, the upper end of the inner pipe communicates with a gas generating device, and the lower end of the inner pipe sealingly connects with an interface of the closed reactor.

[0012] Water inlets and water outlets are arranged at both ends of the shell layer and both ends of the outer pipe, the water inlets are connected with a constant-temperature water bath box through pump bodies, and the water outlets are connected to the constant-temperature water bath box through pipelines.

[0013] The stirring paddle of the stirring device is located in the closed reactor.

[0014] The interface of the closed reactor is provided with a plug valve.

[0015] Two plug valves are sequentially arranged on the joint from top to bottom.

[0016] One end of the balance pipe penetrates through the shell layer and is connected to the pipe wall of the tube layer below the feeding hopper of the liquid raw material dropper, and the other end is connected to the pipe wall of the joint below the plug valve.

[0017] One end of the balance pipe is connected to the pipe wall of the tube layer below the feeding hopper of the liquid raw material dropper, and the other end is connected to the pipe wall between the two plug valves of the joint.

[0018] The gas generating device comprises a gas storage bottle, a first gas distribution pipe, a second gas distribution pipe, a first valve, and a dryer sequentially communicating with the outlet of the gas storage bottle through pipelines, the outlet end of the dryer communicates with the first gas distribution pipe through a gas conveying pipe, the first gas distribution pipe and the second gas distribution pipe are both arranged with equal numbers of corresponding branch pipes at equal intervals along the length direction, one pair of branch pipes of the first gas distribution pipe and the second gas distribution pipe form a group and respectively communicate with two interfaces of a three-way valve, the other interface of the three-way valve communicates with the upper end of the inner pipe of the protective gas inputter, the second gas distribution pipe further communicates with a gas pump, and the first gas distribution pipe further communicates with a bubbling device.

[0019] A thermometer and a pressure gauge are installed in the closed reactor.

[0020] The outer wall of the constant-temperature water bath box is wrapped with heat insulation material. Compared with the prior art, the beneficial effects of the utility model lie in that: through the comprehensive reaction device, balanced and efficient chemical reaction process can be realized, zirconium tetrachloride is added through a solid feeder, diethylamine is added dropwise through a liquid raw material dropping device, cyclopentadiene is added dropwise through a liquid raw material dropping device, nitrogen is input through a protective gas input device, raw materials can be added to the reactor under the condition of air and water isolation, the feeding speed of the liquid raw material dropping device and the solid raw material feeder can be controlled, the input of the reaction raw materials is balancedly controlled, the chemical reaction is continuously promoted under the environment atmosphere full of protective gas, and the reaction efficiency and product yield are improved. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 It is a schematic diagram of the overall reaction device;

[0022] Figure 2 It is a structural schematic diagram of the solid raw material feeder;

[0023] Figure 3 It is a structural schematic diagram of the protective gas input device;

[0024] Figure 4 It is a schematic diagram of the gas generating device;

[0025] Figure 5 It is a structural schematic diagram of the liquid raw material dropping device;

[0026] Figure 6 It is a structural schematic diagram of the liquid raw material dropping device. DETAILED DESCRIPTION

[0027] The drawings are only used for illustrative description, and cannot be understood as the limitation of the present application; in order to better illustrate the embodiment, some components in the drawings can be omitted, enlarged or reduced, and do not represent the size of the actual product; for those skilled in the art, it is understandable that some known structures and their descriptions in the drawings can be omitted; the position relationship described in the drawings is only used for illustrative description, and cannot be understood as the limitation of the present application. The present application will be further described in detail below in combination with specific embodiments.

[0028] As Figure 1As shown, the utility model discloses a kind of reaction device for preparing dichloride dimethylzirconium, including constant temperature water bath box 1, and the closed reactor 2 in constant temperature water bath box 1, multiple interfaces are provided on closed reactor 2, one solid raw material feeder 4, two liquid raw material dropwise feeders 8 and protective gas inputter 5, and stirring device 3, closed reactor 2 first adds initial solvent: ethylene glycol dimethyl ether (1,2-dimethoxyethane), one liquid raw material dropwise feeder 8 is used to dropwise add diethylamine to closed reactor 2, another liquid raw material dropwise feeder 8 is used to dropwise add cyclopentadiene monomer to closed reactor 2, solid raw material feeder 4 is used to add zirconium tetrachloride to closed reactor 2 by gram, protective gas inputter 5 is connected with connecting gas generation device 6, can input inert gas.Closed reactor 2 prepares dichloride dimethylzirconium in it.

[0029] As Figure 1 As shown, closed reactor 2 is box-shaped, and multiple interfaces are provided on its upper end, including first interface and third interface communicated with two liquid raw material dropwise feeders 8, second interface communicated with protective gas inputter 5, fourth interface communicated with solid raw material feeder 4, and fifth interface inserted with thermometer 7, wherein first interface, second interface, third interface, fourth interface and fifth interface are all opened on the upper end face of closed reactor 2, so as to vertically install two liquid raw material dropwise feeders 8, solid raw material feeder 4 and protective gas inputter 5 on closed reactor 2.The upper end face of closed reactor 2 is also centrally provided with stirring device 3, the stirring rod of stirring device 3 penetrates the aperture on the upper end face of closed reactor 2, the lower end of the stirring rod is provided with stirring paddle, and the upper end of the stirring rod is coaxially connected with the output shaft of stirring motor, so that the stirring paddle in closed reactor 2 can be rotated by starting the stirring motor, so that the materials in closed reactor 2 are uniformly mixed.

[0030] Constant temperature water bath box 1 is semi-open box-shaped, closed reactor 2 can be placed in constant temperature water bath box 1, and there is space reserved for the side wall of constant temperature water bath box 1, ice water mixture is pre-stored in constant temperature water bath box 1 as the medium of water bath, and a proper amount of ice and cold water are mixed in constant temperature water bath box 1, so as to provide a stable 0°C environment. With the progress of the reaction, the ice may melt, and ice is added regularly to keep the reaction temperature of closed reactor 2 stable. Outside constant temperature water bath box 1, the outer wall surface of constant temperature water bath box 1 is wrapped with heat insulation material (such as foam, thermal insulation cotton, etc.), so as to reduce heat loss or absorption. A thermometer is arranged in constant temperature water bath box 1, for monitoring the temperature of water bath, if the temperature of water bath deviates from 0°C, the temperature can be restored by adding ice. The medium in constant temperature water bath box 1 can also be replaced by other liquids, so that constant temperature water bath box 1 can keep a lower reaction temperature for closed reactor 2.

[0031] As Figure 2The diagram shows the structure of the solid raw material feeder 4, which includes a raw material pipe 41, a feed pipe 43, and a constant pressure pipe 45. The raw material pipe 41 is used to hold zirconium tetrachloride for the reaction. The raw material pipe 41 is a long and thin tube with a feed hopper 47 at its upper end and a stopcock. The lower end is connected to the feed pipe 43, which is arranged horizontally. The left end of the feed pipe 43 and the portion below the feed hopper 47 of the raw material pipe 41 are connected by two sections of a constant pressure pipe 45. The lower end of the constant pressure pipe 45 is provided with a downward-facing, unsealed discharge port 44, which is used for a sealed connection with the interface of the closed reactor 2. The right end of the feed pipe 43 is provided with a rotating handle 46, which is pivotally connected to the spiral auger 48 inside the feed pipe 43. The feed pipe 43 and the spiral auger 48 are rotatably connected. Zirconium tetrachloride in the raw material pipe 41 falls into the spiral auger 48. The rotating handle 46 can push the spiral auger 48 to discharge the zirconium tetrachloride into the discharge port 44. Controlling the number of rotations of the rotating handle 46 can control the speed at which the raw material in the spiral auger 48 is pushed into the discharge port 44. The solid raw material feeder 4 is equipped with a constant pressure pipe 45, which maintains the air pressure balance in the raw material pipe 41 and the spiral auger 48 to facilitate the smooth falling of the raw material. When the reactants are filled into the feed pipe 41 and the feed hopper 47 is blocked by the stopcock, it facilitates the smooth falling of the reactants.

[0032] like Figure 3 The diagram shows the structure of the protective gas input device 5, which includes an inner tube 51 and an outer tube 52. The upper end of the inner tube 51 is connected to the gas generating device 6, and the lower end of the inner tube 51 can be connected to the second interface of the sealed reactor 2. An outer tube 52 is fitted onto the outer wall of the inner tube 52. The length of the outer tube 52 is less than the length of the inner tube 51, and the upper and lower edges of the outer tube 52 are respectively closed to the tube wall of the inner tube 51, so that a closed cavity is formed between the outer tube 52 and the inner tube 51. A second water inlet 53 and a second water outlet 54 are opened on the side walls at both ends of the outer tube 52. The second water inlet 53 is located below the second water outlet 54. The second water inlet 53 is connected to the constant temperature water bath 1 through a water pump, and the second water outlet 54 returns cooling water to the constant temperature water bath 1 through a pipeline. This ensures that when gas is input into the sealed reactor 2, the organic matter volatilized in the sealed reactor 2 is condensed and refluxed.

[0033] like Figure 5As shown in the structural schematic diagram of the liquid raw material dropping device 8, the tube layer 81 is used to contain the raw material (diethylamine or cyclopentadiene monomer) for reaction, and the shell layer 82 has a medium flowing therein for cooling, so that the dropped reaction raw material is maintained at a constant temperature. The tube layer 81 is in an elongated tubular shape, has a feeding hopper 47 arranged at the upper end thereof and is provided with a plug, and has a plug valve 86 arranged at the lower end thereof, and the plug valve 86 is below a discharge port, and the discharge port of the tube layer 81 can be connected to the first interface and the third interface of the sealed reactor 2. The rotation angle of the plug valve 86 can be controlled to control the dropping speed of the raw material in the tube layer 81. The side wall of the tube layer 81 is provided with a balance pipe 85, one end of the balance pipe 85 is communicated with the tube layer 81 below the feeding hopper 47 of the liquid raw material dropping device 8, and the other end of the balance pipe 85 is communicated with the tube layer 81 below the plug valve 86 through the shell layer 82. When the reaction raw material is filled in the tube layer 81 and the feeding hopper 47 of the liquid raw material dropping device 8 is blocked by the plug, the balance pipe 85 is arranged to facilitate the smooth dropping of the raw material, so that the air pressure in the tube layer 81 is balanced to facilitate the smooth dropping of the raw material. The shell layer 82 is also in an elongated tubular shape, the shell layer 82 is sleeved on the outer periphery of the tube layer 81, the length of the shell layer 82 is less than that of the tube layer 81, the upper edge of the shell layer 82 is closed connected to the pipe wall of the tube layer 81 below the feeding hopper 47 of the liquid raw material dropping device 8, and the lower edge of the shell layer 82 is closed connected to the pipe wall of the tube layer 81 above the plug valve 86, so that a closed cavity is formed between the shell layer 82 and the tube layer 81; the water inlet one 83 and the water outlet one 84 are respectively arranged on the side walls at both ends of the shell layer 82, the water inlet one 83 is below the water outlet one 84, the water inlet one 83 is connected to the constant-temperature water bath box 1 through a water pump, and the water outlet one 83 sends the cooling water back to the constant-temperature water bath box 1 through a pipeline, so that the dropped reaction raw material and the reactants in the sealed reactor 2 are at the same temperature, which can promote the reaction process and improve the reaction efficiency.

[0034] Optionally, the solid raw material feeder 4, the liquid raw material dropping device 8 and the protective gas input device 5 are made of transparent materials.

[0035] As Figure 4As shown, it is a schematic diagram of the gas generating device 6, including a gas cylinder 61, a dryer 64, a three-way valve 69, two gas distribution pipes and a gas pump 67 and a bubbling device 68. The first gas distribution pipe 70 and the second gas distribution pipe 71 are both arranged with equal number of corresponding branches equidistantly along the length direction, and a pair of branches of the first gas distribution pipe 70 and the second gas distribution pipe 71 constitutes a group, and each group of branches is communicated with two interfaces of the three-way valve 69, and the third interface of the three-way valve 69 is communicated with the upper end of the inner pipe 51 of the protective gas input device 5. Specifically, the gas cylinder includes two gas cylinders, one of which 61 stores inert gas such as nitrogen or argon, and the other stores reaction gas. The gas cylinder 61 is connected with the dryer 64 through a valve 62, and a flow meter 63 is arranged between the valve 62 and the dryer 64 for monitoring the gas flow and adjusting the opening of the valve 62 in time to adjust the gas delivery amount and control the gas composition ratio. The outlet end of the dryer 64 is communicated with the first gas distribution pipe 70 through a gas conveying pipe 66, and the second gas distribution pipe 71 is also communicated with the gas pump 67, and the first gas distribution pipe 70 is also communicated with the bubbling device 68.

[0036] Further, according to the reaction needs, a plurality of gas cylinders can also be arranged in communication with the first gas distribution pipe 70, so as to input different kinds of gas into the closed reactor, and adjust the valve 62 of each gas cylinder 61 to adjust the gas flow size delivered into the protective gas input device 5 and the closed reactor 2, so as to adjust the gas composition ratio.

[0037] The use process of the device is as follows: before the reaction starts, the constant temperature water bath box 1 is not in use, the closed reactor 2 is filled with transparent solvent: ethylene glycol dimethyl ether (1, 2-dimethoxyethane), the second interface of the closed reactor 2 is installed with the protective gas input device 5, the first interface, the third interface and the fourth interface of the closed reactor 2 are sealed with a film, and the protective gas input device 5 is communicated with the gas generating device.

[0038] First step: exclude the gas in the reaction device, close the rotary three-way valve 69, so that the closed reactor 2 is communicated with the gas pump 67 through the second gas distribution pipe 71, at the same time the closed reactor 2 is disconnected with the first gas distribution pipe 70, and start the gas pump 67 to pump out the gas in the closed reactor 2.

[0039] Second step: fill inert gas into the reaction device, rotate the three-way valve 69, so that the closed reactor 2 is disconnected with the second gas distribution pipe 71, at the same time the closed reactor 2 is communicated with the gas cylinder 61 containing inert gas and the bubbling device 68 through the first gas distribution pipe 70, and fill inert gas into the closed reactor 2 until the bubbling device 68 starts to bubble. Repeat the steps of the first step and the second step, and repeat the gas replacement operation until the gas in the closed reactor 2 and the connecting pipeline is replaced.

[0040] Third, keep the protective gas nitrogen gas supplied from the gas storage cylinder 61 containing inert gas to the closed reactor 2, and observe the bubbles bubbling out of the bubbling device 68. Start the constant temperature water bath and keep the temperature below 80 degrees Celsius. At the same time, insert the discharge port 44 of the solid raw material feeder 4, which has been loaded with the reaction raw material zirconium tetrachloride, into the fourth interface of the closed reactor 2. Open the stopcock of the feed hopper 47 of the solid raw material feeder 4 and connect the feed hopper of the solid raw material feeder 4 to the bubbling device 68 through the hose. Continue to supply protective gas to replace the gas in the solid raw material feeder 4. Finally, clamp the hose with a clamp and then turn the rotating handle 46 to make the spiral auger 48 in the feed pipe 43 rotate, so that the solid zirconium tetrachloride in the raw material pipe 41 falls into the closed reactor 2.

[0041] Fourth step: Maintain the inert gas storage cylinder 61 by supplying the protective gas (nitrogen) to the sealed reactor 2, and observe the bubbles forming in the bubbling device 68. Start the constant temperature water bath and maintain the temperature below 80 degrees Celsius. Simultaneously, insert the outlets of the liquid feed dropper 8 (containing diethylamine and cyclopentadiene monomer) into the first and third ports of the sealed reactor 2, respectively. Open the stopcock of the feed hopper 47 of the liquid feed dropper 8 and allow the liquid feed... The feed hopper of the dropper 8 is connected to the bubbling device 68 via a hose. Protective gas is continuously introduced to replace the gas in the liquid raw material dropper 8. Finally, the hose is clamped, and then the stopcock valve 86 is turned to add water-white liquid (diethylamine) and colorless transparent liquid (cyclopentadiene monomer) dropwise into the closed reactor 2. At the same time, transparent nitrogen gas is continuously introduced into the closed reactor 2. The reaction is carried out in a water bath for 10-15 hours. Zirconium tetrachloride reacts with diethylamine and cyclopentadiene to produce zirconium dichlorocerochloride, and the solution turns white.

[0042] In this embodiment, the injection of raw materials by the solid raw material feeder 4 and the liquid raw material dripper 8 is completed in an air-isolated operating box. After the raw materials are loaded into the solid raw material feeder 4 and the liquid raw material dripper 8, the discharge port 44 and the outlet are sealed with plastic film. No air or water is introduced into the solid raw material feeder 4 and the liquid raw material dripper 8.

[0043] This embodiment Figure 5 The first gas distribution pipe 70 and the second gas distribution pipe 71 are equipped with multiple pairs of branch pipes to facilitate the connection of multiple closed reactors 2 through three-way valves, so as to allow for intermittent operation and increase production.

[0044] In this embodiment, no air or water is introduced into the reaction process in the closed reactor 2. The amount of raw materials added is finely adjusted by the stopcock valve 66 and the rotating handle 46 to control the reaction temperature.

[0045] Furthermore, such as Figure 6The improved liquid raw material dropper 8 is shown, the part of the pipe layer 81 after penetrating the lower end of the shell layer 82 is sequentially provided with two plug valves 86 from top to bottom, one end of the balance pipe 85 is communicated with the pipe layer 81 below the feeding hopper 87 of the liquid raw material dropper 8, the other end penetrates the shell layer 82 and is communicated with the pipe layer 81 between the two plug valves 86, and other structures of the liquid raw material dropper 8 are the same as Figure 5 The liquid raw material dropper 8 in the utility model is used, the lower end of the liquid raw material dropper 8 injected with the reaction raw material and sealing the upper end of the feeding hopper is directly inserted into the first interface and the third interface of the sealed reactor 2, then the two plug valves 86 are sequentially opened, and the liquid reaction raw material can be added, and the step of replacing the gas is omitted. Figure 6

[0046] Figure 5 Figure 6 The liquid raw material dropper 8 in the utility model is used, the lower end of the liquid raw material dropper 8 injected with the reaction raw material and sealing the upper end of the feeding hopper is directly inserted into the first interface and the third interface of the sealed reactor 2, then the two plug valves 86 are sequentially opened, and the liquid reaction raw material can be added, and the step of replacing the gas is omitted.

[0047] The reaction device can also be used for preparing tris (dimethylamine) cyclopentadienyl zirconium, when the reaction device is used for preparing tris (dimethylamine) cyclopentadienyl zirconium, n-hexane is first loaded into the sealed reactor 2, one liquid raw material dropper 8 is used for adding n-butyl lithium, another liquid raw material dropper 8 is used for adding cyclopentadiene monomer, the solid raw material feeder 4 is used for adding zirconium tetrachloride, the protective gas input device 5 is simultaneously connected with the gas cylinder 61 containing dimethylamine and the gas cylinder containing protective gas through the gas generating device 6, the constant temperature water bath box 1 keeps the temperature below 0 DEG C, then tris (dimethylamine) cyclopentadienyl zirconium can be prepared according to the preparation method disclosed in CN116751232A.

[0048] Compared with the prior reaction device CN116751232A, the reaction device has the advantages that the structure is simple, the amount of reaction raw material can be finely controlled, the reaction temperature can be controlled, and air and water can be avoided in the feeding process. Through the comprehensive reaction device, the balanced and efficient chemical reaction process can be realized, on one hand, the solid raw material is fed to the reaction material through the raw material dropper, on the other hand, the protective gas and the reaction gas are input into the reaction container through the protective gas input device, which can avoid the escape of volatile chemical substances, balance the input of the reaction raw material, and continuously promote the chemical reaction in the environment full of protective gas, thereby improving the reaction efficiency and the product yield.​​

Claims

1. A reaction apparatus for preparing bis-cyclopentadienyl zirconium dichloride comprising a closed reactor (2) disposed in a thermostatic water bath (1), said closed reactor (2) being equipped with a stirring device (7) and a plurality of interfaces, characterized in that, The closed reactor (2) is provided with a solid material feeder (4), two liquid material drop feeders (8) and a protective gas input device (5); The solid material feeder (4) comprises a material pipe (41), a feeding pipe (43) and a constant pressure pipe (45), the upper end of the material pipe (41) is configured as a feeding hopper (47) with a plug, the lower end of the material pipe (41) is connected to the transversely arranged feeding pipe (43), one end of the feeding pipe (43) is connected to the lower end of the constant pressure pipe (45), the upper end of the constant pressure pipe (45) is connected to the upper part of the material pipe (41), and the lower end of the constant pressure pipe (45) is provided with a downwardly open but not closed discharge port (44) for sealed connection with the interface of the closed reactor (2); The other end of the feeding pipe (43) is provided with a rotating handle (46), the rotating handle (46) is pivotally connected to a spiral auger (48) in the feeding pipe (43), and the feeding pipe (43) is rotationally connected to the spiral auger (48). The liquid material drop feeder (8) comprises a pipe layer (81) and a shell layer (82) sleeved on the outer wall of the pipe layer (81), a cavity filled with flowing cooling medium is formed between the pipe layer (81) and the shell layer (82), the upper end of the pipe layer (81) extending out of the shell layer (82) is configured as a feeding hopper (47) with a plug, a plug valve (86) is arranged at the middle part of the lower end of the pipe layer (81) extending out of the shell layer (82), a joint of the pipe layer (81) below the plug valve (86) is used for sealed connection with the interface of the closed reactor (2), one end of a balance pipe (85) penetrates through the shell layer (82) and is connected to the side wall of the pipe layer (81), and the other end of the balance pipe (85) is connected to the side wall of the joint below the plug valve (86).

2. The reaction apparatus according to claim 1, wherein The interfaces communicating with the solid material feeder (4) and the liquid material drop feeder (8) and the interface communicating with the protective gas input device (5) are all arranged on the upper end surface of the closed reactor (2).

3. The reaction apparatus of claim 1, wherein The protective gas input device (5) comprises an inner pipe (51) and an outer pipe (52) sleeved on the outer wall of the inner pipe (51), a cavity filled with flowing cooling medium is formed between the inner pipe (51) and the outer pipe (52), the upper end of the inner pipe (51) is connected to a gas generating device (6), and the lower end of the inner pipe (51) is connected to the interface of the closed reactor (2) in a sealed manner. Water inlets and water outlets are arranged at the two ends of the shell layer (82) and the two ends of the outer pipe (52), the water inlets are connected to a constant temperature water bath box (1) through pump bodies, and the water outlets are connected to the constant temperature water bath box (1) through pipelines. The stirring paddle of the stirring device (7) is located in the closed reactor (2).

4. The reaction apparatus of claim 1, wherein Plug valves are arranged on the interfaces of the closed reactor (2).

5. The reaction apparatus of claim 1, wherein Two plug valves (86) are arranged on the joint from top to bottom.

6. The reaction apparatus of claim 5, wherein One end of the balance pipe (85) penetrates through the shell layer (82) and is connected to the pipe wall of the pipe layer (81) below the feeding hopper (47) of the liquid material drop feeder (8), and the other end of the balance pipe (85) is connected to the pipe wall of the joint below the plug valve (86).

7. The reaction apparatus of claim 6, wherein One end of the balance pipe (85) is connected to the pipe wall below the feed hopper (47) of the liquid raw material drop feeder (8) of the pipe layer (81), and the other end is connected to the pipe wall between the two plug valves (86) of the joint.

8. The reaction apparatus of claim 3, wherein The gas generating device (6) comprises a gas cylinder (61), a first gas distribution pipe (70), a second gas distribution pipe (71), a first valve (62) sequentially communicating with the outlet of the gas cylinder (61) through a pipeline, a dryer (64), the outlet end of the dryer (64) being communicated with the first gas distribution pipe (70) through a gas conveying pipe (66), the first gas distribution pipe (70) and the second gas distribution pipe (71) being equidistantly arranged along the length direction and having equal number of corresponding branch pipes, a pair of branch pipes of the first gas distribution pipe (70) and the second gas distribution pipe (71) forming a group and being communicated with two interfaces of a three-way valve (69) respectively, another interface of the three-way valve (69) being communicated with the upper end of an inner pipe (51) of the protective gas input device (5), the second gas distribution pipe (71) being further communicated with a gas pump (67), and the first gas distribution pipe (70) being further communicated with a bubbling device (68).

9. The reactor of claim 1 wherein, The closed reactor (2) is provided with a thermometer and a pressure gauge.

10. The reaction apparatus of claim 1, wherein The outer wall surface of the constant-temperature water bath box (1) is wrapped with heat insulation material.

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