Device and method for preparing bis (triphenylphosphine) palladium dichloride

Abstract

The invention relates to the field of chemical production, and discloses a preparation device and method of bis (triphenylphosphine) palladium dichloride, the preparation device comprises a base, the top of the base is fixedly connected with a preparation cylinder, the front end of the preparation cylinder is fixedly connected with a window, and the top of the preparation cylinder is fixedly connected with a motor; the device comprises a preparation cylinder, the top of the preparation cylinder is fixedly connected with an arc-shaped supporting plate, the inner wall of the preparation cylinder is rotatably connected with a stirring rod, the outer side of the arc-shaped supporting plate is fixedly connected with a quantifying mechanism, the quantifying mechanism comprises a quantifying cylinder, and the outer wall of the quantifying cylinder is fixedly connected with the outer wall of the arc-shaped supporting plate. And the inner wall of the quantifying cylinder is in sliding connection with a partition plate. By arranging the quantifying mechanism, the adding amount of chemical agents can be accurately controlled, and the inner wall space of the three groups of quantifying cylinders is adjusted according to the total manufacturing amount, so that the quantifying effect is achieved, the proportion of the chemical agents is accurately controlled, and the problem that the adding amount is difficult to accurately control in a traditional mode is solved.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, in particular to a preparation device and a method of bistriphenylphosphine palladium dichloride. Background Art

[0002] In the field of chemistry, bis(triphenylphosphine)palladium dichloride is an important catalyst widely used in organic synthesis reactions. Its efficient catalytic performance enables many complex chemical reactions to be carried out under relatively mild conditions, thereby improving the reaction yield and selectivity.

[0003] In the production process of bistriphenylphosphine palladium dichloride, a preparation cylinder is needed, and the raw materials are first poured into the inner wall of the preparation cylinder, and then a variety of different chemical agents are added to the raw materials, so as to utilize the different characteristics of the chemical agents to produce chemical reactions, and then the chemical agents are fully mixed with the raw materials by stirring to form the finished bistriphenylphosphine palladium dichloride.

[0004] Considering that in the process of adding chemicals, workers usually pour the chemicals into the preparation barrel for mixing at one time, the following problems are prone to occur: first, it is difficult to accurately control the amount of chemicals added, which affects the progress of the reaction and the quality of the final product; second, in the process of re-mixing, a complete dose of chemicals is directly added to the raw materials at one time, which may easily lead to the complete dose of chemicals being unable to be fully mixed with the raw materials, further affecting the quality of the finished product. Summary of the invention

[0005] In view of the shortcomings of the prior art, the present invention provides a preparation device and method for bistriphenylphosphine palladium dichloride, which solves the problems in the production of bistriphenylphosphine palladium dichloride, that is, in the traditional method of manually pouring chemical agents into a preparation barrel for mixing at one time, it is difficult to accurately control the amount of addition, which affects the reaction process and product quality, and the chemical agents cannot be fully mixed with the raw materials, which further affects the quality of the finished product.

[0006] To achieve the above objectives, the present invention is implemented through the following technical solutions: a preparation device for bistriphenylphosphine palladium dichloride, comprising a base, a preparation cylinder fixedly connected to the top of the base, a viewing window fixedly connected to the front end of the preparation cylinder, a motor fixedly connected to the top of the preparation cylinder, an arc-shaped support plate fixedly connected to the top of the preparation cylinder, a stirring rod rotatably connected to the inner wall of the preparation cylinder, a quantitative mechanism fixedly connected to the outer side of the arc-shaped support plate, the quantitative mechanism comprising a quantitative cylinder, the outer wall of the quantitative cylinder is fixedly connected to the outer wall of the arc-shaped support plate, a partition plate is slidably connected to the inner wall of the quantitative cylinder, a threaded rod is rotatably connected to the top of the partition plate, a discharge pipe is fixedly connected to the bottom of the quantitative cylinder, the outer wall of the discharge pipe penetrates the inner wall of the preparation cylinder and is fixedly connected, the outer wall of the quantitative cylinder is fixedly connected to a liquid inlet pipe, a control mechanism is provided on the threaded rod, and a uniform discharge mechanism is provided on the discharge pipe.

[0007] Preferably, a blade is fixedly connected to the outer wall of the stirring rod, and the top outer wall of the blade is arranged in an arc shape.

[0008] Preferably, a sealing rubber ring is fixedly connected to the inner wall of the partition plate, and the outer wall of the sealing rubber ring is connected to the inner wall piston of the quantitative cylinder.

[0009] Preferably, the control mechanism includes an arc-shaped plate, the inner wall of the arc-shaped plate is penetrated by and fixedly connected with an outer rod, the outer wall of the arc-shaped plate is fixedly connected with a sliding block, the top of the metering cylinder is fixedly connected with a sliding track, the inner wall of the sliding track is fixedly connected with a guide rod, and the outer wall of the guide rod is penetrated by and slidably connected with the inner wall of the sliding block.

[0010] Preferably, the outer wall of the outer rod passes through the top of the quantitative cylinder and is slidably connected, and the inner wall of the outer rod is threadedly connected to the outer wall of the threaded rod.

[0011] Preferably, a fastening bolt is threadedly connected to the outer wall of the sliding block, and the outer wall of the fastening bolt is in contact with the outer wall of the sliding track.

[0012] Preferably, the uniform drainage mechanism includes a sealing ball, the bottom of the sealing ball fits with the bottom of the inner wall of the drainage pipe, the bottom of the sealing ball is fixedly connected to a connecting rod, the bottom of the connecting rod is fixedly connected to an arc block, and the inner wall of the metering cylinder is fixedly connected to a support plate.

[0013] Preferably, the inner wall of the support plate penetrates and is slidably connected to the outer wall of the connecting rod.

[0014] Preferably, the bottom of the support plate is fixedly connected to one end of the spring, and the other end of the spring is fixedly connected to the top of the arc block.

[0015] A method for using a bistriphenylphosphine palladium dichloride preparation device comprises the following steps:

[0016] S1. First, according to the total amount of bistriphenylphosphine palladium dichloride to be produced, determine the amount of chemical agents to be added, rotate the fastening bolts outward to release the fitting and fixing effect of the fastening bolts on the sliding track, and move the arc plate vertically, so that the arc plate drives the outer rod to move vertically, and use the self-locking effect of the threaded rod to move the partition plates in the three groups of quantitative cylinders vertically at the same time, and change the inner wall space of the three groups of quantitative cylinders at the same time, so as to achieve the effect of controlling and adjusting the total amount of chemical agents according to the total amount of production;

[0017] S2. At the same time, when the ratio of the three groups of chemicals needs to be adjusted, the staff rotates the threaded rod of one group separately, so that the threaded rod rotates vertically along the inner wall of the outer rod, and at the same time drives the bottom partition plate to move vertically for a second time, so that the position of one group of partition plates is changed separately, so as to adjust the dosage ratio of one of the chemical agents separately;

[0018] S3. After all the chemicals are poured into the quantitative cylinder, the staff closes the feed pipe to ensure the amount of chemicals in the quantitative cylinder, and starts the motor to drive the stirring rod to rotate. During the process of the stirring rod rotating along the inner wall of the preparation cylinder, the top outer wall of the stirring rod will produce an extrusion effect on the bottom of the arc block, so that the arc block drives the connecting rod to move vertically through extrusion, so that the connecting rod drives the sealing ball to extend upward along the inner wall of the discharge pipe, so that the sealing ball releases the sealing effect on the bottom outlet of the discharge pipe, and the chemicals in the quantitative cylinder are discharged downward, so that during the stirring process, the chemicals are added to the raw materials in batches for mixing, which further ensures the uniformity of mixing;

[0019] S4. After the preparation cylinder completes the mixing and stirring of the liquid, the finished product in the preparation cylinder is taken out through the discharge pipe, and the finished product is heated and dried using a dryer. The heating time is 5-6 hours and the heating temperature is 80-100°C, thereby obtaining the finished product of bistriphenylphosphine palladium dichloride.

[0020] The present invention provides a device and method for preparing bistriphenylphosphine palladium dichloride.

[0021] Beneficial effects:

[0022] 1. The present invention can accurately control the amount of chemical agents added by setting a quantitative mechanism, and adjust the inner wall space of the three groups of quantitative cylinders according to the total production amount, so as to achieve a quantitative effect, accurately control the proportion of chemical agents, and solve the problem that it is difficult to accurately control the amount of addition in the traditional way.

[0023] 2. The present invention uses the design of the threaded rod to ensure the accuracy of the ratio and increase or decrease the overall dosage of the chemical agents. It can also adjust one of the chemical agents separately according to the formula, further improving the adaptability of the device and solving the problem that it is difficult to accurately control the ratio in the traditional way.

[0024] 3. The present invention uses a uniform liquid discharge mechanism. During the stirring process, the stirring rod squeezes the arc block to move the sealing ball, so that the chemical agents are added to the raw materials in batches for mixing, avoiding the problem of insufficient mixing caused by adding a complete dose of chemical agents at one time, and further improving the quality of the finished product. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 A perspective view of the present invention;

[0026] Figure 2 It is a schematic diagram of the cross-sectional structure of the preparation tube of the present invention;

[0027] Figure 3 It is a schematic diagram of the cross-sectional structure of the metering cylinder of the present invention;

[0028] Figure 4 It is a schematic diagram of the structure of the sliding track and the guide rod of the present invention;

[0029] Figure 5 It is a schematic diagram of the control mechanism structure of the present invention;

[0030] Figure 6 For the present invention Figure 5 The enlarged structural diagram of part A in the middle;

[0031] Figure 7 The figure is a flow chart of the method for using the present invention.

[0032] Among them, 1. base; 2. preparation cylinder; 3. window; 4. arc-shaped support plate; 5. motor; 6. stirring rod; 7. quantitative mechanism; 701. quantitative cylinder; 702. partition plate; 703. discharge pipe; 704. liquid inlet pipe; 705. threaded rod; 8. uniform discharge mechanism; 801. sealing ball; 802. connecting rod; 803. arc-shaped block; 804. spring; 9. control mechanism; 901. arc-shaped plate; 902. sliding track; 903. fastening bolt; 904. slider; 905. guide rod; 906. outer rod. DETAILED DESCRIPTION

[0033] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Example:

[0035] Please see attached Figure 1 - Attachment Figure 7 The embodiment of the present invention provides a preparation device of bistriphenylphosphine palladium dichloride, comprising a base 1, a preparation tube 2 is fixedly connected to the top of the base 1, so that the base provides a supporting and fixing effect for the preparation tube 2 to ensure its stability during use, a window 3 is fixedly connected to the front end of the preparation tube 2, through which the liquid and raw materials in the inner wall of the preparation tube 2 can be observed, a motor 5 is fixedly connected to the top of the preparation tube 2, so that the preparation tube 2 provides a supporting and fixing effect for the motor 5, an arc-shaped support plate 4 is fixedly connected to the top of the preparation tube 2, so that the preparation tube 2 provides a supporting and fixing effect for the arc-shaped support plate 4, the inner wall of the preparation tube 2 is rotatably connected with a stirring rod 6, the output shaft of the motor 5 is fixedly connected to the top of the stirring rod 6, and by starting the motor 5, the motor 5 drives the stirring rod 6 to rotate, thereby achieving the effect of mixing and stirring the raw materials and liquid in the inner wall of the preparation tube 2, and the outer wall of the stirring rod 6 is fixedly connected with blades, and the top outer wall of the blade is arranged in an arc shape.

[0036] The outer side of the arc-shaped support plate 4 is fixedly connected with a quantitative mechanism 7, and the quantitative mechanism 7 includes a quantitative cylinder 701. The outer wall of the quantitative cylinder 701 is fixedly connected to the outer wall of the arc-shaped support plate 4, so that the arc-shaped support plate 4 provides a supporting and fixing effect for the quantitative cylinder 701. The inner wall of the quantitative cylinder 701 is slidably connected with a partition plate 702. Through the design of the partition plate 702, the inner wall of the quantitative cylinder 701 is separated, thereby achieving a quantitative effect, and the outer wall of the quantitative cylinder 701 is engraved with a measurement value, and the quantitative cylinder 701 is transparent, which is convenient for the staff to observe the position of the partition plate 702 in the inner wall of the quantitative cylinder 701. The inner wall of the partition plate 702 is fixedly connected with a sealing rubber ring, and the outer wall of the sealing rubber ring is connected to the inner wall piston of the quantitative cylinder 701, so as to further improve the sealing effect between the partition plate 702 and the inner wall of the quantitative cylinder 701.

[0037] The top of the partition plate 702 is rotatably connected to a threaded rod 705, so that the threaded rod 705 drives the partition plate 702 to move vertically. The bottom of the quantitative cylinder 701 is fixedly connected to a drain pipe 703, through which the liquid in the inner wall of the quantitative cylinder 701 is discharged downward. The outer wall of the drain pipe 703 penetrates the inner wall of the preparation cylinder 2 and is fixedly connected. The outer wall of the quantitative cylinder 701 is fixedly connected to a liquid inlet pipe 704, through which the external liquid is transmitted to the inner wall of the quantitative cylinder 701 for storage. A control mechanism 9 is arranged on the threaded rod 705, and the control mechanism 9 includes an arc Plate 901, the inner wall of the arc plate 901 passes through and is fixedly connected with an outer rod 906, so that the arc plate 901 drives the outer rod 906 to move vertically at the same time during the vertical movement, the outer wall of the outer rod 906 passes through the top of the metering cylinder 701 and is slidably connected to maintain the stability of the vertical movement of the outer rod 906, the inner wall of the outer rod 906 is threadedly connected to the outer wall of the threaded rod 705, so that the threaded rod 705 moves vertically along the inner wall of the outer rod 906, and the outer wall of the arc plate 901 is fixedly connected with a slider 904, so that the arc plate 901 drives the slider 904 to move vertically at the same time during the vertical movement.

[0038] The top of the metering cylinder 701 is fixedly connected to a sliding track 902, and the inner wall of the sliding track 902 is fixedly connected to a guide rod 905. The outer wall of the guide rod 905 penetrates and is slidably connected to the inner wall of the slider 904, keeping the slider 904 moving vertically along the guide rod 905 and the inner wall of the sliding track 902. The outer wall of the slider 904 is threadedly connected to a fastening bolt 903, and the slider 904 is fixed by the fastening bolt 903 to maintain the vertical position of the arc plate 901. The outer wall of the fastening bolt 903 is in contact with the outer wall of the sliding track 902.

[0039] The drain pipe 703 is provided with a uniform drain mechanism 8, which includes a sealing ball 801. The bottom of the sealing ball 801 fits with the bottom of the inner wall of the drain pipe 703 to achieve the effect of sealing the bottom of the drain pipe 703. The bottom of the sealing ball 801 is fixedly connected with a connecting rod 802, and the bottom of the connecting rod 802 is fixedly connected with an arc block 803, so that the arc block 803 moves vertically and drives the connecting rod 802 to move at the same time, so that the connecting rod 802 drives the sealing ball 801 to move vertically at the same time, and quantitative The inner wall of the cylinder 701 is fixedly connected to a support plate, so that the inner wall of the quantitative cylinder 701 provides a supporting and fixing effect for the support plate. The inner wall of the support plate penetrates and is slidably connected to the outer wall of the connecting rod 802, thereby maintaining the stability of the vertical movement of the connecting rod 802. The bottom of the support plate is fixedly connected to one end of the spring 804, and the other end of the spring 804 is fixedly connected to the top of the arc block 803, so that the arc block 803 is driven downward by the force of the spring 804, so that the sealing ball 801 always maintains a fixing effect on the discharge pipe 703.

[0040] A method for using a bistriphenylphosphine palladium dichloride preparation device comprises the following steps:

[0041] S1. First, according to the total amount of bistriphenylphosphine palladium dichloride to be produced, determine the amount of chemical agents to be added, rotate the fastening bolts 903 outward to release the fastening bolts 903 from the fitting and fixing effect on the sliding track 902, and move the arc plate 901 vertically, so that the arc plate 901 drives the outer rod 906 to move vertically, and use the self-locking effect of the threaded rod 705 to make the partition plates 702 in the three groups of quantitative cylinders 701 move vertically at the same time, and change the inner wall space of the three groups of quantitative cylinders 701 at the same time, so as to achieve the effect of controlling and adjusting the total amount of chemical agents according to the total amount of production;

[0042] S2. At the same time, when the ratio of the chemical agents in the three groups needs to be adjusted, the staff rotates the threaded rod 705 of one group separately, so that the threaded rod 705 rotates vertically along the inner wall of the outer rod 906, and drives the bottom partition plate 702 to move vertically for a second time, so that the position of one group of partition plates 702 is changed separately, and the dosage ratio of one of the chemical agents is adjusted separately, so that the device can ensure the accuracy of the ratio, increase or reduce the overall dosage of the chemical agents, and can also adjust one of the chemical agents separately according to the formula, further improving the adaptability of the device;

[0043] S3. After all the chemicals are poured into the quantitative cylinder 701, the staff closes the liquid inlet pipe 704 to ensure the amount of chemicals in the quantitative cylinder 701, and starts the motor 5, so that the motor 5 drives the stirring rod 6 to rotate. During the process of the stirring rod 6 rotating along the inner wall of the preparation cylinder 2, the top outer wall of the stirring rod 6 will produce an extrusion effect on the bottom of the arc block 803, so that the arc block 803 drives the connecting rod 802 to move vertically by extrusion, so that the connecting rod 802 drives the sealing ball 801 to extend upward along the inner wall of the discharge pipe 703, so that the sealing ball 801 releases the sealing effect on the bottom outlet of the discharge pipe 703, and the chemicals in the quantitative cylinder 701 are discharged downward, so that during the stirring process, the chemicals are added to the raw materials in batches for mixing, which further ensures the uniformity of mixing;

[0044] S4. After the preparation cylinder 2 completes the mixing and stirring of the liquid, the finished product in the preparation cylinder 2 is taken out through the discharge pipe, and the finished product is heated and dried using a dryer. The heating time is 6 hours and the heating temperature is 80° C., thereby obtaining the finished product of bistriphenylphosphine palladium dichloride.

[0045] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A preparation device for bistriphenylphosphine palladium dichloride, characterized in that, The invention comprises a base (1), the top of the base (1) is fixedly connected to a preparation cylinder (2), the front end of the preparation cylinder (2) is fixedly connected to a viewing window (3), the top of the preparation cylinder (2) is fixedly connected to a motor (5), the top of the preparation cylinder (2) is fixedly connected to an arc-shaped support plate (4), the inner wall of the preparation cylinder (2) is rotatably connected to a stirring rod (6), the outer side of the arc-shaped support plate (4) is fixedly connected to a quantitative mechanism (7), the quantitative mechanism (7) comprises a quantitative cylinder (701), the outer wall of the quantitative cylinder (701) and the arc-shaped support plate (4) are connected to each other. The outer wall is fixedly connected, the inner wall of the quantitative cylinder (701) is slidably connected to a partition plate (702), the top of the partition plate (702) is rotatably connected to a threaded rod (705), the bottom of the quantitative cylinder (701) is fixedly connected to a discharge pipe (703), the outer wall of the discharge pipe (703) penetrates the inner wall of the preparation cylinder (2) and is fixedly connected, the outer wall of the quantitative cylinder (701) is fixedly connected to a liquid inlet pipe (704), the threaded rod (705) is provided with a control mechanism (9), and the discharge pipe (703) is provided with a uniform discharge mechanism (8).

2. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 1, characterized in that, The outer wall of the stirring rod (6) is fixedly connected with a blade, and the top outer wall of the blade is arranged in an arc shape.

3. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 1, characterized in that, A sealing rubber ring is fixedly connected to the inner wall of the partition plate (702), and the outer wall of the sealing rubber ring is connected to the inner wall piston of the metering cylinder (701).

4. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 1, characterized in that, The control mechanism (9) comprises an arc-shaped plate (901), the inner wall of the arc-shaped plate (901) penetrates and is fixedly connected to an outer rod (906), the outer wall of the arc-shaped plate (901) is fixedly connected to a sliding block (904), the top of the metering cylinder (701) is fixedly connected to a sliding track (902), the inner wall of the sliding track (902) is fixedly connected to a guide rod (905), and the outer wall of the guide rod (905) penetrates and is slidably connected to the inner wall of the sliding block (904).

5. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 4, characterized in that, The outer wall of the outer rod (906) passes through the top of the quantitative cylinder (701) and is slidably connected, and the inner wall of the outer rod (906) is threadedly connected to the outer wall of the threaded rod (705).

6. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 4, characterized in that, The outer wall of the sliding block (904) is threadedly connected with a fastening bolt (903), and the outer wall of the fastening bolt (903) is in contact with the outer wall of the sliding track (902).

7. A preparation device for a bistriphenylphosphine palladium chloride according to claim 1, characterized in that, The uniform liquid discharge mechanism (8) comprises a sealing ball (801), the bottom of the sealing ball (801) is in contact with the bottom of the inner wall of the liquid discharge pipe (703), the bottom of the sealing ball (801) is fixedly connected to a connecting rod (802), the bottom of the connecting rod (802) is fixedly connected to an arc block (803), and the inner wall of the quantitative cylinder (701) is fixedly connected to a support plate.

8. A preparation device for a bistriphenylphosphine palladium chloride according to claim 1, characterized in that, The inner wall of the support plate penetrates and is slidably connected to the outer wall of the connecting rod (802).

9. The preparation device of a kind of bistriphenylphosphine palladium dichloride according to claim 1, characterized in that, The bottom of the support plate is fixedly connected to one end of the spring (804), and the other end of the spring (804) is fixedly connected to the top of the arc block (803).

10. The method for preparing a bistriphenylphosphine palladium dichloride according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. First, the amount of chemical agent to be added is determined according to the total amount of bistriphenylphosphine palladium dichloride to be produced, and the fastening bolt (903) is rotated outward to release the fastening bolt (903) from the fitting and fixing effect on the sliding track (902), and the arc plate (901) is moved vertically, so that the arc plate (901) drives the outer rod (906) to move vertically, and the self-locking effect of the threaded rod (705) is used to move the partition plates (702) in the three groups of quantitative cylinders (701) vertically at the same time, and the inner wall space of the three groups of quantitative cylinders (701) is changed at the same time, so as to achieve the effect of controlling and adjusting the total amount of chemical agents according to the total amount produced; S2. At the same time, when the chemical ratios in the three groups need to be adjusted, the staff rotates the threaded rod (705) of one group separately, so that the threaded rod (705) is rotated vertically along the inner wall of the outer rod (906), and the bottom partition plate (702) is driven to perform a secondary vertical movement, so that the position of one group of partition plates (702) is changed separately; S3. After all the chemicals are poured into the quantitative cylinder (701), the staff closes the liquid inlet pipe (704) to ensure the amount of chemicals in the quantitative cylinder (701), and starts the motor (5) so that the motor (5) drives the stirring rod (6) to rotate. During the process of the stirring rod (6) rotating along the inner wall of the preparation cylinder (2), the top outer wall of the stirring rod (6) produces an extrusion effect on the bottom of the arc block (803), so that the arc block (803) drives the connecting rod (802) to move vertically by extrusion, so that the connecting rod (802) drives the sealing ball (801) to extend upward along the inner wall of the discharge pipe (703), so that the sealing ball (801) releases the sealing effect on the bottom outlet of the discharge pipe (703), and the chemicals in the quantitative cylinder (701) are discharged downward; S4. After the preparation cylinder (2) completes the mixing and stirring of the liquid, the finished product in the preparation cylinder (2) is taken out through the discharge pipe, and the finished product is heated and dried using a dryer. The heating time is 5-6 hours and the heating temperature is 80-100° C., thereby obtaining the finished product of bistriphenylphosphine palladium dichloride.

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