Palladium chloride concentration and crystallization device

Abstract

The utility model discloses a palladium chloride concentration crystallization device which comprises a rack, a machine head, a flask, a water bath heating structure, a transfer pipe, a feeding pipe, a condenser and a collecting bottle: a split type connecting structure is adopted, the flask comprises a straight line section connected with the machine head, one side, far away from the machine head, of the straight line section is connected with a flask section, and the pipe diameter of the straight line part of the flask section is smaller than that of the straight line section; the split type connecting structure comprises a sealing cylinder nested on the outer side of the straight line part of the flask section, a sealing net is arranged at the opening of the flask section, the outer side of the straight line section and the outer side of the flask section are wrapped with a sealing rubber sleeve, the outer side of the sealing rubber sleeve is movably sleeved with a pressure dividing assembly, and the bottom of the pressure dividing assembly extends and is fixed to the outer side of the water bath heating structure; when the machine head rotates, the straight line section is driven to rotate, the flask section is driven to rotate on the inner side of the pressure dividing assembly through the straight line section, and a user does not need to worry about falling of the flask even if the flask is communicated with the atmosphere on the premise that a motor is not stopped.

Description

Technical Field

[0001] The utility model relates to palladium chloride preparation equipment, in particular to a palladium chloride concentration and crystallization device. Background Art

[0002] Palladium chloride is an inorganic compound used to prepare special catalysts and molecular sieves. Its preparation process involves complexing dichlorodiammine palladium with ammonia water, followed by filtration after reduction with hydrazine hydrate to obtain a primary product, which is then subjected to chlorination leaching and secondary filtration. The filtered product is concentrated and crystallized to obtain palladium chloride. During the concentration and crystallization process, the solution is mainly evaporated and crystallized using a rotary evaporator. The filtered solution is introduced into a flask, which is rotated at a constant speed and heated. The volatile solvent is continuously distilled under reduced pressure to obtain palladium chloride.

[0003] During the concentration process of the rotary evaporator, the flask needs to be kept in a negative pressure state before it can rotate to prevent the flask from falling. However, when some novice operators operate the equipment, they often forget to let in atmospheric pressure before turning off the power structure, which causes the flask to fall and the remaining liquid in it to spill, which is quite troublesome. Utility Model Content

[0004] The utility model provides a palladium chloride concentration crystallization device, which can better ensure the stability of the flask. Even if the atmosphere is ventilated under the premise that the motor has not stopped, there is no need to worry about the flask falling off, and the above-mentioned problem can be effectively solved.

[0005] The utility model is achieved in this way:

[0006] A palladium chloride concentration crystallization device comprises a frame, a machine head is provided on the frame, a flask is connected to one side of the machine head, a water bath heating structure is provided at the lower end of the flask, a transfer pipe is connected to the other side of the machine head, the transfer pipe is communicated with a feed pipe, a condenser is provided at the upper end of the feed pipe, and a collecting bottle is connected to the lower end of the feed pipe.

[0007] A split connection structure, the flask includes a straight section connected to the machine head, the straight section is connected to a flask section on the side away from the machine head, the diameter of the straight part of the flask section is smaller than the straight section, the split connection structure includes a sealing cylinder nested on the outside of the straight section of the flask section, a sealing net is provided at the opening of the flask section, the outside of the straight section and the flask section are wrapped with a closed rubber sleeve, the outer movable sleeve of the closed rubber sleeve is provided with a pressure dividing assembly, the bottom of the pressure dividing assembly extends and is fixed to the outside of the water bath heating structure, when the machine head rotates, the straight section is driven to rotate, and the flask section is driven to rotate on the inside of the pressure dividing assembly through the straight section.

[0008] As a further improvement, the sealing cylinder includes an inner sealing section located between the straight section and the straight portion of the flask section, and a flat-mouth section is provided on the outer edge of the opening of the flask section. The flat-mouth section and the inner sealing section are integrally formed.

[0009] As a further improvement, the sealing rubber sleeve is a convex structure, and the sealing rubber sleeve includes a large sealing portion sleeved outside the straight section and a small sealing portion sleeved outside the straight section of the flask section.

[0010] As a further improvement, the pressure dividing assembly includes a first bearing and a second bearing which are sleeved on the outside of the large closed part and the small closed part. A solid cylinder is fixed on the outside of the first bearing and the second bearing, and the solid cylinder is extended and fixed to the outside of the water bath heating structure through an extension bracket.

[0011] As a further improvement, the solid cylinder includes a first fixing frame adapted to the outer side of the first bearing, and a second fixing frame adapted to the outer side of the second bearing, and the first fixing frame and the second fixing frame form a convex structure.

[0012] As a further improvement, the mounting tube includes a reducing tube fixed to the sealing net, a flow tube is provided on the side of the reducing tube away from the sealing net, a plurality of holes are provided on the outside of the reducing tube and the flow tube, and the end of the flow tube is connected to the storage rack.

[0013] The beneficial effects of the utility model are:

[0014] In the existing concentration and crystallization equipment, the anti-boiling material is directly located in the flask, and the flask is directly connected to the machine head. In this way, during the operation of a novice, if the machine head is connected to the atmosphere before it stops running, the flask is prone to malfunctions such as falling off and falling. Therefore, the utility model divides the original entire flask into segments, namely a straight line segment and a flask segment, and sets a split connection structure at the connection position between the two. First, a sealing cylinder is set on the outside of the straight part of the flask segment, so that the flask segment can fit tightly with the outside of the straight line segment. At the same time, the outside of the entire straight line segment and the flask segment are fixed by a closed rubber sleeve, so that the two can fit tightly together without leakage. The closed rubber sleeve is pressure-bearing through the pressure-dividing component, so that even if the straight line segment is separated from the machine head, the entire straight line segment and the flask segment can be tightly supported by the pressure-dividing component, thereby preventing the flask from directly falling off and being damaged. Even if the straight line segment and the flask segment are forcibly separated, the flask segment can be supported by the pressure-dividing component to achieve double protection.

[0015] In order to allow the flask segment with a smaller diameter to cooperate with the straight segment, thereby preventing the evaporated gas from leaking out, the utility model provides an integrated inner sealing segment and a flat-mouth segment on the outside of the straight portion of the flask segment, that is, between the flask segment and the straight segment. Therefore, after the flask segment is embedded in the straight segment, it is not easy to slide and breathe. Even if the inner sealing segment is subjected to tension, it will involve the flat-mouth segment, and the overall sealing performance is greatly improved.

[0016] After the sealing cylinder is provided, even if the flask segment and the inner side of the straight segment form a good sealing effect, if only this segment is used for sealing, air leakage will easily occur after the sealing part of this segment ages. Therefore, the utility model provides a sealing rubber sleeve on the basis of the sealing cylinder. The sealing parts at both ends of the sealing rubber sleeve are fixed in steps, and the two sealing parts are connected to achieve the outer side sealing. Combined with the inner side sealing, a two-stage seal is formed. Even if one part of it ages after long-term use, it is not easy to leak on a large scale.

[0017] During the entire concentration process, the equipment needs to be kept in a reduced pressure state, and then the machine head is started to rotate the entire flask. If positive pressure is directly introduced without stopping the machine head, it is easy to cause the flask to fall out. Therefore, the utility model is provided with two bearings on the basis of the sealing cylinder and the sealing rubber sleeve, which respectively fix the two sections of pipes with different diameters. On the outside of the two bearings, a solid cylinder is separately provided for protection and fixation. The solid cylinder is located in the middle of the flask section and the straight section. Therefore, no matter whether the straight section itself is separated from the machine head or the straight section is separated from the flask section, it will not affect the stability of the flask section at the rear section of the flask, thereby ensuring that the flask section will not fall off and be damaged. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following is a brief introduction to the drawings required for use in the embodiments. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without creative work.

[0019] Figure 1 It is a structural schematic diagram (first perspective) of a palladium chloride concentration and crystallization device of the present invention.

[0020] Figure 2 It is a structural schematic diagram of a palladium chloride concentration and crystallization device of the present invention (second viewing angle).

[0021] Figure 3 The utility model is a schematic diagram of the top structure of a palladium chloride concentration and crystallization device.

[0022] Figure 4 This utility model Figure 3 Cross-section view at AA in the middle.

[0023] Figure 5 This utility model Figure 4 Magnified view of area B.

[0024] Figure 6 It is a structural schematic diagram of the cooperation between the flask and the split-type connecting structure of the utility model.

[0025] Figure 7 This utility model Figure 6 Schematic diagram of the top view structure.

[0026] Figure 8 This utility model Figure 7 Isometric section at mid-CC.

[0027] Figure 9 It is a structural schematic diagram of the water bath heating structure of the utility model.

[0028] In the picture:

[0029] Frame 10, machine head 20, flask 30, straight section 31, flask section 32, water bath heating structure 40, heating furnace 41, oblique ring plate 42, output pump 43, central ball 44, transfer pipe 50, feed pipe 60, condenser 70, collecting bottle 80, split connection structure 1, sealing cylinder 101, inner sealing section 1011, flat section 1012, sealing net 102, sealing rubber sleeve 103, large sealing part 1031, small sealing part 1032, pressure dividing assembly 104, first bearing 1041, second bearing 1042, solid cylinder 1043, first fixing frame 10431, second fixing frame 10432, extension bracket 1044, installation cylinder 201, reducing tube 2011, circulation tube 2012, storage rack 202, lower sealing bowl 2021, upper sealing bowl 2022. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the utility model for which protection is sought, but merely represents the selected embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0031] In the description of this utility model, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of the technical features indicated. Therefore, a feature specified as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of this utility model, "plurality" means two or more, unless otherwise specifically specified.

[0032] Reference Figures 1 to 9As shown, a palladium chloride concentration and crystallization device comprises a frame 10, on which an organic head 20 is provided, one side of the machine head 20 is connected to a flask 30, the lower end of the flask 30 is provided with a water bath heating structure 40, the other side of the machine head 20 is connected to a transfer tube 50, the transfer tube 50 is communicated with a feed pipe 60, the upper end of the feed pipe 60 is provided with a condenser 70, the lower end of the feed pipe 60 is connected to a collecting bottle 80, characterized in that the concentration and crystallization equipment further comprises: a split connection structure 1, the flask 30 comprises a straight section 31 connected to the machine head 20, the side of the straight section 31 away from the machine head 20 is connected to a flask section 32, the diameter of the straight section of the flask section 32 is smaller than the straight section 31, the split connection structure 1 comprises a sealing cylinder 101 nested on the outside of the straight section of the flask section 32, a sealing net 102 is provided at the opening of the flask section 32, the The outside of the straight segment 31 and the flask segment 32 is wrapped with a closed rubber sleeve 103, and the outer movable sleeve of the closed rubber sleeve 103 is provided with a pressure dividing assembly 104, the bottom of the pressure dividing assembly 104 extends and is fixed to the outside of the water bath heating structure 40, and when the head 20 rotates, it drives the straight segment 31 to rotate, and drives the flask segment 32 to rotate inside the pressure dividing assembly 104 through the straight segment 31; the cantilevered containing structure includes a mounting tube 201 arranged on the inner side of the sealing net 102, the mounting tube 201 is tightly attached to the inner side of the straight part of the flask segment 32, and the end of the mounting tube 201 is connected to a storage rack 202, the storage rack 202 is cantilevered in the circular cavity of the flask segment 32, the interior of the storage rack 202 is filled with anti-boiling particles, the storage rack 202 is immersed in the liquid in the flask segment 32, and when the flask segment 32 rotates, it drives the storage rack 202 and the anti-boiling particles in the storage rack 202 to rotate.

[0033] During the entire concentration and crystallization process, the palladium chloride liquid is first added to the flask 30 through the feed pipe 60 and the transfer pipe 50. Then, the internal environment of the entire flask 30 is depressurized, and the head 20 is driven to rotate. At the same time, the water bath heating structure 40 is started to evaporate the liquid in the flask 30. The evaporated gas flows through the condenser 70 for cooling, flows into the collecting bottle 80, and is discharged to obtain palladium chloride.

[0034] The sealing net 102 is a filter screen that can filter out some impurities.

[0035] In the existing concentrated crystallization equipment, the anti-boiling material is directly located in the flask 30, and the flask 30 is directly connected to the machine head 20. In this way, during the operation of a novice, if the machine head 20 is not yet stopped and is connected to the atmosphere, the flask 30 is prone to malfunctions such as falling off or falling. Therefore, the utility model divides the original entire flask 30 into segments, divided into a straight line segment 31 and a flask segment 32, and sets a split connection structure 1 at the connection position between the two. First, a sealing cylinder 101 is set on the outside of the straight part of the flask segment 32, so that the flask segment 32 can be tightly connected to the outside of the straight line segment 31. The straight section 31 and the flask section 32 are tightly fitted together. At the same time, the outer sides of the straight section 31 and the flask section 32 are fixed by a closed rubber sleeve 103, so that the two can fit together tightly without air leakage, and the closed rubber sleeve 103 is pressure-bearing through the pressure-dividing component 104. Therefore, even if the straight section 31 is separated from the machine head 20, the entire straight section 31 and the flask section 32 can be tightly supported by the pressure-dividing component 104, thereby preventing the flask 30 from falling off and being damaged directly. Even if the straight section 31 and the flask section 32 are forcibly separated, the flask section 32 can be supported by the pressure-dividing component 104, thereby achieving double protection.

[0036] In order to allow the flask segment 32 with a smaller diameter to cooperate with the straight segment 31, thereby preventing the evaporated gas from leaking, the sealing cylinder 101 of this embodiment includes an inner sealing segment 1011 located between the straight segment 31 and the straight part of the flask segment 32, and a flat-mouth segment 1012 is provided on the outer edge of the opening of the flask segment 32. The flat-mouth segment 1012 and the inner sealing segment 1011 are integrally formed, and an integrated inner sealing segment 1011 and flat-mouth segment 1012 are provided on the outside of the straight part of the flask segment 32, that is, between the flask segment 32 and the straight segment 31. Therefore, after the flask segment 32 is embedded in the straight segment 31, it is not easy to slide and breathe. Even if the inner sealing segment 1011 is subjected to tension, it will involve the flat-mouth segment 1012, and the overall sealing performance is greatly improved.

[0037] After the sealing cylinder 101 is provided, even if the flask segment 32 and the inner side of the straight segment 31 form a good sealing effect, if only this segment is used for sealing, air leakage will easily occur after the sealing part of this segment ages. Therefore, the sealing rubber sleeve 103 of this embodiment is a convex structure, and the sealing rubber sleeve 103 includes a large sealing portion 1031 sleeved on the outside of the straight segment 31 and a small sealing portion 1032 sleeved on the outside of the straight portion of the flask segment 32. The sealing rubber sleeve 103 is provided on the basis of the sealing cylinder 101. The sealing portions at both ends of the sealing rubber sleeve 103 are fixed in steps, and the two sections of the sealing portions are connected, thereby achieving sealing on the outside. Combined with the sealing on the inside, a two-stage seal is formed. Even if one part of it ages after long-term use, large-scale leakage is not likely to occur.

[0038] During the entire concentration process, the device needs to be kept in a decompressed state before the machine head 20 is started to rotate the entire flask 30. If the machine head 20 is not stopped and positive pressure is directly introduced, it is easy to cause the flask 30 to fall out. Therefore, the pressure dividing assembly 104 of this embodiment includes a first bearing 1041 and a second bearing 1042 that are sleeved on the outside of the large closing portion 1031 and the small closing portion 1032. A solid cylinder 1043 is fixed to the outside of the first bearing 1041 and the second bearing 1042. The solid cylinder 1043 is connected to the outside of the large closing portion 1031 and the small closing portion 1032 by an extension bracket 1044. It extends and is fixed to the outside of the water bath heating structure 40. Two bearings are provided on the basis of the sealing cylinder 101 and the sealing rubber sleeve 103 to fix the two sections of pipes with different calibers respectively. On the outside of the two bearings, a solid cylinder 1043 is separately provided for protection and fixation. The solid cylinder 1043 is located in the middle of the flask segment 32 and the straight segment 31. Therefore, no matter whether the straight segment 31 itself is separated from the machine head 20 or the straight segment 31 is separated from the flask segment 32, it will not affect the stability of the flask segment 32 at the rear section of the flask 30, thereby ensuring that the flask segment 32 will not fall off and be damaged.

[0039] In order to adapt to bearings of different sizes and provide support for them, the solid cylinder 1043 includes a first fixing frame 10431 that is adapted to the outer side of the first bearing 1041, and a second fixing frame 10432 that is adapted to the outer side of the second bearing 1042. The first fixing frame 10431 and the second fixing frame 10432 form a convex structure, which adaptively positions and fixes the first bearing 1041 and the second bearing 1042. The extended bracket 1044 on the outer side of the solid cylinder 1043 adopts a ring and L-shaped bracket, which is the existing technology and will not be described in detail here.

[0040] During the rotation of the flask 30, the liquid therein will form a liquid film, thereby increasing the heating area of the liquid and making it more sufficient during evaporation. However, if anti-boiling particles are added to the flask 30, the liquid film will be destroyed as the flask 30 rotates, affecting the heating area. Therefore, the utility model provides a mounting cylinder 201 at the position of the sealing net 102 on the basis of the split connection structure 1. The mounting cylinder 201 extends to the interior of the flask 30 through a storage rack 202. The anti-boiling particles are stored in the storage rack 202. The storage rack 202 is in a cantilevered state in the flask 30, that is, it does not contact any inner wall surface of the flask 30. When the storage rack 202 and the mounting cylinder 201 rotate with the flask 30, the anti-boiling particles will always be at the bottom of the entire storage rack 202 and in contact with the solution in the flask 30, thereby being able to stop the boiling of the liquid while avoiding the destruction of the liquid film in the flask 30.

[0041] Among them, in order to avoid obstructing the normal circulation of gas and at the same time improve the coordination effect between the installation tube 201 and the straight part of the flask section 32, the installation tube 201 includes a reducing tube 2011 fixedly connected to the sealing net 102, and a flow tube 2012 is provided on the side of the reducing tube 2011 away from the sealing net 102. A plurality of holes are provided on the outer sides of the reducing tube 2011 and the flow tube 2012, and the end of the flow tube 2012 is connected to the storage rack 202. The holes provided in the reducing tube 2011 and the flow tube 2012 can make the evaporated gas circulate more freely, and the clamping coordination effect of the reducing tube 2011, the flow tube 2012 and the flask section 32 can make the storage rack 202 more stable.

[0042] The anti-boiling particles are stored in a storage rack 202. In order to allow the liquid to come into contact with the anti-boiling particles, the storage rack 202 of this embodiment includes a lower sealing bowl 2021 connected to the circulation tube 2012. An upper sealing bowl 2022 is locked above the lower sealing bowl 2021. The lower sealing bowl 2021 and the upper sealing bowl 2022 form a space for accommodating the anti-boiling particles. The surface of the storage rack 202 is configured to have a lower sealing bowl 2021 and an upper sealing bowl 2022 with holes. The lower sealing bowl 2021 and the upper sealing bowl 2022 are fixed in an openable and closable manner, thereby facilitating the filling and replacement of the anti-boiling particles.

[0043] When the flask section 32 is heated in a water bath, not all parts of the flask section 32 containing the solution are in contact with water, and a large part of the part is not in contact with water. Therefore, the water bath heating structure 40 of this embodiment includes a heating furnace 41 for heating the liquid, and an inclined ring plate 42 is provided on the upper edge of the heating furnace 41, which is inclined inward. A number of output pumps 43 are installed on the inner side of the inclined ring plate 42, and a central ball 44 is provided in the middle of the furnace body of the heating furnace 41. The central ball 44 is connected to a number of output pumps 43 through a number of pipes. Through the additional water bath heating structure 40, the water at the bottom of the heating furnace 41 can be pumped upward and pressed onto the outer wall of the flask section 32 through the output pump 43 on the inclined ring plate 42, so that the part of the flask section 32 that is not in direct contact with water can also receive a better heating effect, thereby achieving the purpose of uniform heating.

[0044] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that the present invention is susceptible to various modifications and variations. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A palladium chloride concentration crystallization device, characterized in that, The machine comprises a frame (10), a head (20) is provided on the frame (10), a flask (30) is connected to one side of the head (20), a water bath heating structure (40) is provided at the lower end of the flask (30), a transfer pipe (50) is connected to the other side of the head (20), the transfer pipe (50) is communicated with a feed pipe (60), a condenser (70) is provided at the upper end of the feed pipe (60), and a collecting bottle (80) is connected to the lower end of the feed pipe (60): The split connection structure (1) comprises a flask (30) comprising a straight section (31) connected to a machine head (20), a flask section (32) being connected to a side of the straight section (31) away from the machine head (20), the diameter of the straight section of the flask section (32) being smaller than that of the straight section (31), the split connection structure (1) comprising a sealing cylinder (101) nested outside the straight section of the flask section (32), a sealing net (101) being provided at the opening of the flask section (32) 2), the outer sides of the straight section (31) and the flask section (32) are wrapped with a closed rubber sleeve (103), and the outer movable sleeve of the closed rubber sleeve (103) is provided with a pressure dividing assembly (104), the bottom of the pressure dividing assembly (104) extends and is fixed to the outer side of the water bath heating structure (40), and when the head (20) rotates, the straight section (31) is driven to rotate, and the flask section (32) is driven to rotate inside the pressure dividing assembly (104) through the straight section (31).

2. a kind of palladium chloride concentrating crystallization device according to claim 1, is characterized in that, The sealing cylinder (101) comprises an inner sealing section (1011) located between the straight section (31) and the straight portion of the flask section (32); a flat-mouth section (1012) is provided on the outer edge of the opening of the flask section (32); the flat-mouth section (1012) and the inner sealing section (1011) are integrally formed.

3. a kind of palladium chloride concentrating crystallization device according to claim 1, is characterized in that, The sealing rubber sleeve (103) is a convex structure, and comprises a large sealing portion (1031) sleeved on the outside of the straight section (31) and a small sealing portion (1032) sleeved on the outside of the straight portion of the flask section (32).

4. a kind of palladium chloride concentrating crystallization device according to claim 3, is characterized in that, The pressure dividing assembly (104) includes a first bearing (1041) and a second bearing (1042) which are sleeved on the outside of the large closed portion (1031) and the small closed portion (1032). A fixed cylinder (1043) is fixed to the outside of the first bearing (1041) and the second bearing (1042). The fixed cylinder (1043) is extended and fixed to the outside of the water bath heating structure (40) through an extension bracket (1044).

5. a kind of palladium chloride concentrating crystallization device according to claim 4, is characterized in that, The solid cylinder (1043) includes a first fixing frame (10431) adapted to the outer side of the first bearing (1041), and a second fixing frame (10432) adapted to the outer side of the second bearing (1042), wherein the first fixing frame (10431) and the second fixing frame (10432) form a convex structure.

6. a kind of palladium chloride concentrating crystallization device according to claim 1, is characterized in that, The sealing net (102) is connected to the installation tube (201), and the installation tube (201) includes a reduced diameter tube (2011) fixedly connected to the sealing net (102). A circulation tube (2012) is provided on the side of the reduced diameter tube (2011) away from the sealing net (102). A plurality of holes are provided on the outer sides of the reduced diameter tube (2011) and the circulation tube (2012), and the end of the circulation tube (2012) is connected to the storage rack (202).

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