A device and method for measuring cyanogen chloride dosage

By designing a cyanide chloride usage measurement device including a reactor, accommodating cylinder and piston cylinder, the inconvenience and error of traditional detection methods are solved, and the accurate measurement of cyanide chloride usage is achieved, providing reliable data support for cyanate ester production.

CN119290105BActive Publication Date: 2025-03-04THE RES INST FOR SPECIAL STRUCTURES OF AERONAUTICAL COMPOSITE AVIC
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Patent Information

Application Number
CN202411848490.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-16
Publication Date
2025-03-04
Estimated Expiration
2044-12-16

AI Technical Summary

Technical Problem

Traditional detection methods are relatively inconvenient to detect the purity of cyanochloride, and the residual cyanochloride in the pipeline during synthesis results in errors in the detection results.

Method used

A cyanochloride consumption measurement device is designed, including a reactor, accommodating cylinder and piston cylinder. By controlling the connection between the reversing valve and the pressure stabilizing tube, the cyanochloride reflux and measurement are achieved to ensure the measurement accuracy.

Benefits of technology

The device can accurately measure the consumption of cyanide chloride, reduce errors, improve measurement convenience and accuracy, and provide reliable data for cyanate production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a device and method for measuring the amount of cyanogen chloride, and belongs to the field of measuring the amount of cyanogen chloride. The device comprises a reactor, wherein a stirrer and a temperature control mechanism are arranged in the reactor, and further comprises a containing cylinder and a piston cylinder with built-in cyanogen chloride, wherein an extraction pipe is connected between the containing cylinder and the piston cylinder, a discharge pipe is connected between the piston cylinder and the reactor, and a first reversing valve and a second reversing valve are respectively arranged on the discharge pipe and the extraction pipe. A piston rod is slidably connected in the piston cylinder, a spring is connected between the piston rod and the piston cylinder, a first voltage-stabilizing tube is connected to the discharge pipe, and a three-way valve is arranged at the connection between the first voltage-stabilizing tube and the discharge pipe. The invention ensures the measurement accuracy, improves the recovery rate of cyanogen chloride, and increases the operation safety by enabling the piston cylinder to transport all the cyanogen chloride remaining in the discharge pipe, the extraction pipe and the piston cylinder back to the containing cylinder after the reaction is completed.
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Description

Technical Field

[0001] The invention relates to the technical field of cyanogen chloride dosage measurement, in particular to a cyanogen chloride dosage measurement device and method. Background Art

[0002] In the chemical industry, cyanogen chloride is an important raw material widely used in the synthesis of chemicals such as cyanate esters. In order to ensure the quality and production efficiency of products such as cyanate esters, it is crucial to accurately control the amount of cyanogen chloride. When synthesizing cyanate esters, the purity of the raw materials will also affect the actual amount of cyanogen chloride. If the raw materials contain impurities, more cyanogen chloride may be needed to compensate for the effects of these impurities on the reaction. Therefore, when replacing different batches of raw materials, it is necessary to test the amount of the raw materials in that batch.

[0003] The traditional detection method is to directly measure the purity of cyanogen chloride and calculate the amount of raw materials to be added in this batch based on the purity. However, measuring the purity of cyanogen chloride requires the use of a large number of additional instruments and additional detection operations, which is cumbersome and inconvenient. Directly measuring the consumption of cyanogen chloride during the synthesis process, the cyanogen chloride remaining in the pipeline will cause errors in the test results. Summary of the invention

[0004] The purpose of the present invention is to provide a device and method for measuring the amount of cyanogen chloride, which solves the problem that it is inconvenient to detect the purity of cyanogen chloride by traditional detection methods, and that the residual cyanogen chloride in the cyanogen chloride dosage pipeline during direct measurement of synthesis leads to errors in the detection results.

[0005] To achieve the above object, the present invention provides the following technical solution: a device for measuring the amount of cyanogen chloride, comprising a reactor, wherein an agitator and a temperature control mechanism are arranged in the reactor, and further comprising a housing cylinder and a piston cylinder with built-in cyanogen chloride, wherein an extraction pipe is connected between the housing cylinder and the piston cylinder, and a discharge pipe is connected between the piston cylinder and the reactor, and a first reversing valve and a second reversing valve are respectively arranged on the discharge pipe and the extraction pipe;

[0006] A piston rod is slidably connected in the piston cylinder, a spring is connected between the piston rod and the piston cylinder, a first voltage-stabilizing tube is connected to the discharge pipe, and a three-way valve is provided at the connection between the first voltage-stabilizing tube and the discharge pipe;

[0007] Before the reaction of cyanogen chloride and bisphenol compound in the reactor is complete, the discharge pipe is not connected with the first voltage-stabilizing tube, the piston cylinder extracts cyanogen chloride in the containing cylinder through the extraction pipe, and discharges the cyanogen chloride into the reactor through the discharge pipe, and, when the reaction of cyanogen chloride and bisphenol compound in the reactor is complete, the discharge pipe is connected with the first voltage-stabilizing tube, and the directions of the first reversing valve and the second reversing valve are changed, so that the piston cylinder transports the cyanogen chloride remaining in the discharge pipe, the extraction pipe and the piston cylinder back to the inside of the containing cylinder.

[0008] Preferably, a pressure valve is provided on the discharge pipe at a position between the three-way valve and the reaction kettle.

[0009] Preferably, it further comprises a mounting platform, the mounting platform is connected to a bracket, the bracket is connected to a motor, the output end of the motor is connected to a rotating shaft, and the bottom end of the rotating shaft is connected to a wobble plate;

[0010] There are two piston cylinders and two piston rods, and the lower surface of the wobble plate is attached to the top ends of the two piston rods.

[0011] Preferably, the rotating shaft is slidably connected to a ring with a key, and the lower surface of the ring is connected to a rack;

[0012] A roller is rotatably connected inside the rotating shaft, a gear meshing with the rack is coaxially connected to the roller, the wobble plate is hinged at the bottom end of the rotating shaft, and an arc strip is connected to the upper surface of the wobble plate, the center trajectory of the arc strip coincides with the swing center of the wobble plate, and the arc strip is fitted to the roller.

[0013] Preferably, a mounting frame is slidably connected to the bracket, an electric telescopic rod is connected to the bottom of the mounting frame, and an output end of the electric telescopic rod is connected to the ring;

[0014] A temperature sensor is arranged in the reactor. When the temperature sensor detects that the temperature in the reactor rises, the electric telescopic rod is shortened to move the ring upward, so that the wobble plate swings toward a horizontal state.

[0015] Preferably, the bracket is slidably connected to a base, the motor is fixedly connected to the base, the base is connected to an electromagnet, the electromagnet is magnetically adsorbed to the bracket, and when the motor stops running or the wobble plate swings to a horizontal state, the electromagnet is powered off.

[0016] Preferably, the outside of the accommodating cylinder is connected to a cooling cylinder, and the cooling cylinder is filled with a refrigerant medium.

[0017] Preferably, the cooling cylinder is connected to a refrigeration pipe, the refrigeration pipe is connected to a water pump, the water pump is fixedly connected to the mounting frame, and the pump shaft of the water pump is fixedly connected to the rotating shaft;

[0018] A refrigeration box is fixedly connected to the mounting platform, and both ends of the refrigeration pipe are connected to the refrigeration box.

[0019] Preferably, a sealing plate is slidably connected inside the accommodating tube, a cover plate is connected to the port cover, and a second voltage-stabilizing tube is penetrated and connected to the cover plate.

[0020] A method for measuring the amount of cyanogen chloride, comprising the following steps:

[0021] S1. Ensure that the reactor, holding cylinder, piston cylinder and related pipelines are well connected, check whether all valves are in the initial state, inject an appropriate amount of cyanogen chloride into the holding cylinder, and ensure that there is sufficient refrigerant in the cooling cylinder;

[0022] S2, start the agitator and temperature control mechanism in the reactor and adjust to the preset reaction conditions;

[0023] S3, injecting cyanogen chloride into the reactor until the cyanogen chloride and the bisphenol compound in the reactor react to reach equilibrium;

[0024] S4, open the three-way valve to connect the discharge pipe with the first voltage-stabilizing pipe, and the discharge pipe is not connected with the reactor at this time, and change the direction of the first reversing valve and the second reversing valve at the same time, so that the cyanogen chloride in the pipeline and the piston cylinder flows back to the containing cylinder;

[0025] S5. After the cyanogen chloride refluxed into the containing cylinder is cooled, observe and record the position change of the sealing plate to calculate the consumption of cyanogen chloride, and record key parameters such as temperature and amount of bisphenol compound during the reaction process to provide a basis for subsequent production.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1. The present invention controls the direction change of the first reversing valve and the second reversing valve, and controls the three-way valve to disconnect the discharge pipe from the reactor, while the discharge pipe is connected to the first voltage-stabilizing tube. At this time, the piston rod slides back and forth in the piston cylinder, so that the cyanogen chloride remaining in the discharge pipe is extracted into the piston cylinder, and the cyanogen chloride in the piston cylinder is then transferred to the containing cylinder through the extraction pipe, until the cyanogen chloride in the discharge pipe, the extraction pipe and the piston cylinder all flows back into the containing cylinder, and then the sliding of the piston rod is stopped, so that the cyanogen chloride consumption in the containing cylinder can be obtained, which provides a basis for the subsequent cyanate ester production. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0029] Figure 2 It is a structural schematic diagram of the rotating shaft of the present invention;

[0030] Figure 3 It is a structural schematic diagram of the wedge plate of the present invention;

[0031] Figure 4 It is a structural schematic diagram of the receiving tube of the present invention;

[0032] Figure 5 It is a structural schematic diagram of the pressure valve of the present invention;

[0033] Figure 6 It is a schematic diagram of the structure of the base of the present invention.

[0034] In the figure: 1. reactor; 2. mounting table; 3. cooling cylinder; 31. containing cylinder; 32. sealing plate; 33. refrigeration pipe; 34. refrigeration box; 35. cover plate; 36. second voltage-stabilizing tube; 4. bracket; 41. rotating shaft; 42. roller; 43. ring; 44. rack; 45. gear; 46. pendulum plate; 47. arc bar; 48. electric telescopic rod; 5. piston cylinder; 51. piston rod; 52. spring; 53. discharge pipe; 531. first reversing valve; 54. extraction pipe; 541. second reversing valve; 55. first voltage-stabilizing tube; 551. three-way valve; 56. pressure valve; 6. motor; 61. base; 62. electromagnet; 63. mounting frame; 64. water pump. DETAILED DESCRIPTION

[0035] The following will be combined with the drawings in the embodiments 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.

[0036] Reference Figure 1-Figure 6The present embodiment provides a technical solution: a device for measuring the amount of cyanogen chloride, comprising a reactor 1, wherein the reactor 1 is provided with an agitator and a temperature control mechanism, and further comprising a housing cylinder 31 and a piston cylinder 5 with built-in cyanogen chloride, wherein an extraction pipe 54 is connected between the housing cylinder 31 and the piston cylinder 5, and a discharge pipe 53 is connected between the piston cylinder 5 and the reactor 1, wherein a first reversing valve 531 and a second reversing valve 541 are respectively provided on the discharge pipe 53 and the extraction pipe 54; a piston rod 51 is slidably connected in the piston cylinder 5, a spring 52 is connected between the piston rod 51 and the piston cylinder 5, a first voltage-stabilizing tube 55 is connected to the discharge pipe 53, and the first voltage-stabilizing tube 55 A three-way valve 551 is provided at the connection with the discharge pipe 53; before the reaction of cyanogen chloride and bisphenol compound in the reactor 1 is complete, the discharge pipe 53 is not connected with the first voltage-stabilizing tube 55, the piston cylinder 5 extracts cyanogen chloride in the accommodating tube 31 through the extraction tube 54, and discharges the cyanogen chloride to the reactor 1 through the discharge pipe 53; and, when the reaction of cyanogen chloride and bisphenol compound in the reactor 1 is complete, the discharge pipe 53 is connected with the first voltage-stabilizing tube 55, the directions of the first reversing valve 531 and the second reversing valve 541 are changed, so that the piston cylinder 5 transports the residual cyanogen chloride in the discharge pipe 53, the extraction pipe 54 and the piston cylinder 5 back to the inside of the accommodating tube 31.

[0037] A certain amount of bisphenol compound is added to the reactor 1, and the agitator and temperature control mechanism in the reactor 1 are started to ensure that the temperature in the reactor 1 is maintained. Cyanogen chloride is injected into the receiving cylinder 31, and the piston rod 51 is controlled to slide back and forth in the piston cylinder 5. When cyanogen chloride is added to the reactor 1, the first reversing valve 531 allows the cyanogen chloride in the piston cylinder 5 to be discharged only through the discharge pipe 53, and the second reversing valve 541 allows the cyanogen chloride to enter the piston cylinder 5 only through the extraction pipe 54, and the three-way valve 551 disconnects the discharge pipe 53 from the first voltage-stabilizing tube 55. At this time, the piston cylinder 5 injects the cyanogen chloride in the receiving cylinder 31 into the reactor 1 to react with the bisphenol compound, and the reaction state of the two is monitored at the same time. When the reaction reaches equilibrium, It is clear that the amount of cyanogen chloride added is sufficient. At this time, the directions of the first reversing valve 531 and the second reversing valve 541 are controlled to change, and the three-way valve 551 is controlled to disconnect the discharge pipe 53 from the reactor 1. At the same time, the discharge pipe 53 is connected to the first voltage-stabilizing tube 55. At this time, the piston rod 51 slides back and forth in the piston cylinder 5, so that the cyanogen chloride remaining in the discharge pipe 53 is extracted into the piston cylinder 5, and the cyanogen chloride in the piston cylinder 5 is then transferred to the containing cylinder 31 through the extraction pipe 54, until the cyanogen chloride in the discharge pipe 53, the extraction pipe 54 and the piston cylinder 5 are all refluxed into the containing cylinder 31, and then the sliding of the piston rod 51 is stopped, so that the amount of cyanogen chloride in the containing cylinder 31 can be measured, and then the consumption of cyanogen chloride can be obtained, which provides a basis for the subsequent production of cyanate esters;

[0038] The reversing valve can be an electromagnetic reversing valve according to the needs. The reaction degree of cyanogen chloride and bisphenol compound can be detected by nuclear magnetic resonance, infrared spectrum, or by reaction temperature deduction.

[0039] Through the above settings, the measurement accuracy is guaranteed, while the recovery rate of cyanogen chloride is improved and the operation safety is increased.

[0040] A pressure valve 56 is provided on the discharge pipe 53 between the three-way valve 551 and the reaction kettle 1 .

[0041] The setting of the pressure valve 56 makes it difficult for the cyanogen chloride in the discharge pipe 53 to flow into the reactor 1 due to gravity, thereby ensuring the precise control of the amount and speed of cyanogen chloride addition, and preventing the cyanogen chloride from entering the reactor 1 due to the increase in temperature and the increase in volume.

[0042] It also includes a mounting platform 2, to which a bracket 4 is connected, to which a motor 6 is connected, to which an output end of the motor 6 is connected a rotating shaft 41, to which a swing plate 46 is connected at the bottom end; there are two piston cylinders 5 and two piston rods 51, and the lower surface of the swing plate 46 is in contact with the top ends of the two piston rods 51.

[0043] When the motor 6 is started, it drives the rotating shaft 41 to rotate, thereby rotating the swing plate 46 connected to the bottom end of the rotating shaft 41. At this time, the swing plate 46 pushes the two piston rods 51 alternately, and the spring 52 resets the piston rod 51. By setting two piston cylinders 5 and the piston rod 51, cyanogen chloride can be continuously introduced into the reactor 1.

[0044] A ring 43 is slidably connected to the rotating shaft 41, and a rack 44 is connected to the lower surface of the ring 43; a roller 42 is rotatably connected inside the rotating shaft 41, and a gear 45 meshing with the rack 44 is coaxially connected to the roller 42; a swing plate 46 is hinged to the bottom end of the rotating shaft 41, and an arcuate bar 47 is connected to the upper surface of the swing plate 46, the center trajectory of the arcuate bar 47 coincides with the swing center of the swing plate 46, and the arcuate bar 47 fits against the roller 42.

[0045] When the ring 43 moves downward, it can drive the rack 44 to move downward synchronously. At this time, the rack 44 drives the gear 45 to rotate, so that the roller 42 rotates. At this time, the roller 42 can drive the arc bar 47 to move under the action of static friction, thereby causing the wobble plate 46 to swing to a horizontal state. When the ring 43 slides down to the lowest point, the wobble plate 46 swings to a horizontal state. Conversely, when the ring 43 moves upward, it drives the wobble plate 46 to swing to an inclined state. By adjusting the inclination of the wobble plate 46, the driven sliding stroke of the piston rod 51 is changed, and the rotation speed of the rotating shaft 41 remains unchanged. Therefore, when the sliding stroke of the piston rod 51 changes, the addition speed of cyanogen chloride is changed.

[0046] A mounting frame 63 is slidably connected to the bracket 4, and an electric telescopic rod 48 is connected to the bottom of the mounting frame 63, and an output end of the electric telescopic rod 48 is connected to the ring 43; a temperature sensor is provided in the reactor 1, and when the temperature sensor detects that the temperature in the reactor 1 rises, the electric telescopic rod 48 shortens to make the ring 43 move upward, so that the swing plate 46 swings toward a horizontal state.

[0047] In order to prevent the reaction between cyanogen chloride and bisphenol compound from being too intense, during the reaction process, the stirrer in the reactor 1 strongly stirs the internal reactants, the temperature control system controls the reaction temperature in the reactor 1 to not fluctuate too much, and the temperature sensor in the reactor 1 continuously monitors the temperature of the internal reactants. When the temperature in the reactor 1 rises, it means that the reaction is too intense and the addition of cyanogen chloride needs to be slowed down or stopped. Thus, the control system controls the electric telescopic rod 48 to extend, and the ring 43 moves downward, so that the swing plate 46 swings toward a horizontal state, so that the sliding stroke of the piston rod 51 is reduced, and the addition speed of cyanogen chloride is further reduced. If the temperature in the reactor 1 continues to increase or increases to a high degree, the electric telescopic rod 48 extends to the longest state, so that the swing plate 46 swings to a horizontal state, so that the swing plate 46 no longer pushes the piston rod 51, and the piston cylinder 5 no longer injects cyanogen chloride into the reactor 1, or the motor 6 stops running.

[0048] In order to prevent the upward section from moving downward and causing the piston rod 51 to be pushed quickly during the swinging of the swing plate 46 to the horizontal state when the swing plate 46 is highly tilted, the directions of the two reversing valves are changed during the extension and retraction of the electric telescopic rod 48, so that the piston cylinder 5 injects cyanogen chloride into the accommodating cylinder 31, thereby preventing the cyanogen chloride in the piston cylinder 5 from being discharged into the reactor 1 during the swinging of the swing plate 46.

[0049] The bracket 4 is slidably connected with a base 61, the motor 6 is fixedly connected to the base 61, the base 61 is connected with an electromagnet 62, the electromagnet 62 is magnetically adsorbed to the bracket 4, and when the motor 6 stops running or the swing plate 46 swings to a horizontal state, the electromagnet 62 is powered off.

[0050] In order to prevent excess cyanogen chloride from entering the reactor 1 when the temperature of cyanogen chloride increases and its volume increases during a violent reaction in the reactor 1, the rotating shaft 41 is adaptively unlocked. Specifically, when the swing plate 46 swings to a horizontal state or the motor 6 stops running, it means that there is no need to continue to add cyanogen chloride to the reactor 1. At this time, the electromagnet 62 is powered off, so that the base 61 can slide relative to the bracket 4. At this time, the temperature of cyanogen chloride in the piston cylinder 5 increases and its volume increases, which can push the piston rod 51 to move upward. After the base 61 is unlocked, it no longer hinders the upward movement of the piston rod 51. In combination with the setting of the pressure valve 56, cyanogen chloride will not expand due to the increase in temperature and enter the reactor 1.

[0051] The outside of the accommodating cylinder 31 is connected to the cooling cylinder 3 , and the cooling cylinder 3 is filled with a refrigerant.

[0052] The cold zone medium in the cooling cylinder 3 keeps the temperature of the cyanogen chloride in the containing cylinder 31 at a constant state, so that the cyanogen chloride in the containing cylinder 31 will not change in volume due to temperature fluctuations, resulting in inaccurate metering of subsequent usage.

[0053] The cooling cylinder 3 is connected to a refrigeration pipe 33, and the refrigeration pipe 33 is connected to a water pump 64. The water pump 64 is fixedly connected to the mounting frame 63, and the pump shaft of the water pump 64 is fixedly connected to the rotating shaft 41; the mounting platform 2 is fixedly connected to a refrigeration box 34, and both ends of the refrigeration pipe 33 are connected to the refrigeration box 34.

[0054] The refrigerant in the refrigeration box 34 is in a constant state. A refrigerator is provided in the refrigeration box 34 to cool the refrigerant. When the motor 6 is running, the water pump 64 is running at the same time. The water pump 64 drives the refrigerant to flow in the cooling cylinder 3 to ensure the temperature control effect on the cyanogen chloride in the containing cylinder 31.

[0055] A sealing plate 32 is slidably connected inside the accommodating tube 31 , and a cover plate 35 is connected to the port cover. A second voltage-stabilizing tube 36 is penetrated and connected to the cover plate 35 .

[0056] The sealing plate 32 is provided so that the cyanogen chloride in the containing tube 31 will not evaporate, which will lead to inaccurate measurement of the subsequent cyanogen chloride dosage. The cover plate 35 improves the heat preservation effect of the containing tube 31. The second voltage regulator tube 36 ensures that the sliding of the sealing plate 32 is not affected by the air pressure.

[0057] After the directions of the two reversing valves are changed so that the cyanogen chloride in the pipeline and the piston cylinder 5 flows back into the containing cylinder 31, the swing plate 46 is controlled to swing to a horizontal state so that the two piston rods 51 no longer slide, but the water pump 64 is in operation. After the cyanogen chloride flowing back into the containing cylinder 31 is cooled, the consumption of cyanogen chloride in the containing cylinder 31 can be obtained, thereby obtaining the amount of cyanogen chloride required for the reaction.

[0058] A method for measuring the amount of cyanogen chloride, comprising the following steps:

[0059] S1. Ensure that the reactor 1, the containing cylinder 31, the piston cylinder 5 and the related pipelines are well connected, check whether all valves are in the initial state, inject an appropriate amount of cyanogen chloride into the containing cylinder 31, and ensure that the refrigerant in the cooling cylinder 3 is sufficient;

[0060] S2, start the agitator and temperature control mechanism in the reactor 1 and adjust them to the preset reaction conditions;

[0061] S3, injecting cyanogen chloride into the reactor 1 until the cyanogen chloride and the bisphenol compound in the reactor 1 react to reach equilibrium;

[0062] S4, open the three-way valve 551 to connect the discharge pipe 53 with the first voltage-stabilizing tube 55. At this time, the discharge pipe 53 is not connected with the reactor 1. At the same time, change the direction of the first reversing valve 531 and the second reversing valve 541 to make the cyanogen chloride in the pipeline and the piston cylinder 5 flow back to the containing cylinder 31;

[0063] S5. After the cyanogen chloride refluxed into the containing tube 31 is cooled, the position change of the sealing plate 32 is observed and recorded to calculate the consumption of cyanogen chloride, and key parameters such as the temperature and the amount of bisphenol compound in the reaction process are recorded to provide a basis for subsequent production.

[0064] 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 device for measuring the amount of cyanogen chloride, comprising a reaction kettle (1), wherein the reaction kettle (1) is provided with a stirrer and a temperature control mechanism, and characterized in that: It also comprises a housing cylinder (31) and a piston cylinder (5) containing cyanogen chloride, an extraction pipe (54) being connected between the housing cylinder (31) and the piston cylinder (5), a discharge pipe (53) being connected between the piston cylinder (5) and the reaction kettle (1), and a first reversing valve (531) and a second reversing valve (541) being respectively provided on the discharge pipe (53) and the extraction pipe (54); A piston rod (51) is slidably connected inside the piston cylinder (5), a spring (52) is connected between the piston rod (51) and the piston cylinder (5), a first voltage-stabilizing tube (55) is connected to the discharge pipe (53), and a three-way valve (551) is provided at the connection between the first voltage-stabilizing tube (55) and the discharge pipe (53); Before the reaction of cyanogen chloride and bisphenol compound in the reactor (1) is complete, the discharge pipe (53) is not connected to the first voltage-stabilizing tube (55), the piston cylinder (5) extracts cyanogen chloride in the containing cylinder (31) through the extraction pipe (54), and discharges the cyanogen chloride into the reactor (1) through the discharge pipe (53); and, when the reaction of cyanogen chloride and bisphenol compound in the reactor (1) is complete, the discharge pipe (53) is connected to the first voltage-stabilizing tube (55), and the directions of the first reversing valve (531) and the second reversing valve (541) are changed, so that the piston cylinder (5) transports the cyanogen chloride remaining in the discharge pipe (53), the extraction pipe (54) and the piston cylinder (5) back to the inside of the containing cylinder (31); A sealing plate (32) is slidably connected inside the containing cylinder (31), and a cover plate (35) is connected to the port cover. A second voltage-stabilizing tube (36) is connected through the cover plate (35). After the cyanogen chloride that flows back into the containing cylinder (31) is cooled, a position change of the sealing plate (32) is observed and recorded to calculate the consumption of cyanogen chloride.

2. The cyanogen chloride dosage measuring device according to claim 1, characterized in that: A pressure valve (56) is provided on the discharge pipe (53) at a location between the three-way valve (551) and the reaction kettle (1).

3. The cyanogen chloride dosage measuring device according to claim 2, characterized in that: It also comprises a mounting platform (2), the mounting platform (2) being connected to a bracket (4), the bracket (4) being connected to a motor (6), the output end of the motor (6) being connected to a rotating shaft (41), and the bottom end of the rotating shaft (41) being connected to a swing plate (46); The number of the piston cylinder (5) and the number of the piston rod (51) are both two, and the lower surface of the swing plate (46) is in contact with the top ends of the two piston rods (51).

4. The cyanogen chloride dosage measuring device according to claim 3, characterized in that: A ring (43) is slidably connected to the upper key of the rotating shaft (41), and a rack (44) is connected to the lower surface of the ring (43); A roller (42) is rotatably connected inside the rotating shaft (41), a gear (45) meshing with the rack (44) is coaxially connected to the roller (42), the swing plate (46) is hinged to the bottom end of the rotating shaft (41), and an arc strip (47) is connected to the upper surface of the swing plate (46), the center trajectory of the arc strip (47) coincides with the swing center of the swing plate (46), and the arc strip (47) is in close contact with the roller (42).

5. The cyanogen chloride dosage measuring device according to claim 4, characterized in that: The bracket (4) is slidably connected to a mounting frame (63), the bottom of the mounting frame (63) is connected to an electric telescopic rod (48), and the output end of the electric telescopic rod (48) is connected to the ring (43); A temperature sensor is provided in the reactor (1). When the temperature sensor detects that the temperature in the reactor (1) rises, the electric telescopic rod (48) is shortened to move the ring (43) upward, thereby causing the swing plate (46) to swing toward a horizontal state.

6. The cyanogen chloride dosage measuring device according to claim 5, characterized in that: The support (4) is slidably connected to a base (61), the motor (6) is fixedly connected to the base (61), the base (61) is connected to an electromagnet (62), the electromagnet (62) is magnetically adsorbed to the support (4), and when the motor (6) stops running or the swing plate (46) swings to a horizontal state, the electromagnet (62) is powered off.

7. The cyanogen chloride dosage measuring device according to claim 6, characterized in that: The outside of the accommodating cylinder (31) is connected to a cooling cylinder (3), and the cooling cylinder (3) is filled with a refrigeration medium.

8. The device for measuring the amount of cyanogen chloride according to claim 7, characterized in that: The cooling cylinder (3) is connected to a refrigeration pipe (33), the refrigeration pipe (33) is connected to a water pump (64), the water pump (64) is fixedly connected to the mounting frame (63), and the pump shaft of the water pump (64) is fixedly connected to the rotating shaft (41); A refrigeration box (34) is fixedly connected to the mounting platform (2), and both ends of the refrigeration pipe (33) are connected to the refrigeration box (34).

9. A method for measuring the amount of cyanogen chloride, applied to the device for measuring the amount of cyanogen chloride according to claim 8, characterized in that: The following steps are involved: S1. Ensure that the reactor (1), the containing cylinder (31), the piston cylinder (5) and related pipelines are connected in good condition, check whether all valves are in their initial state, inject an appropriate amount of cyanogen chloride into the containing cylinder (31), and ensure that the refrigerant in the cooling cylinder (3) is sufficient; S2, starting the agitator and temperature control mechanism in the reaction kettle (1) and adjusting them to the preset reaction conditions; S3, injecting cyanogen chloride into the reaction kettle (1) until the reaction of cyanogen chloride and bisphenol compound in the reaction kettle (1) reaches equilibrium; S4, opening the three-way valve (551) to connect the discharge pipe (53) to the first voltage-stabilizing pipe (55), at which point the discharge pipe (53) is not connected to the reaction kettle (1), and at the same time changing the directions of the first reversing valve (531) and the second reversing valve (541) to allow the cyanogen chloride in the pipeline and the piston cylinder (5) to flow back to the containing cylinder (31); S5. After the cyanogen chloride that has refluxed into the containing tube (31) is cooled, the position change of the sealing plate (32) is observed and recorded to calculate the consumption of cyanogen chloride, and key parameters such as the temperature and the amount of bisphenol compound during the reaction are recorded to provide a basis for subsequent production.

Citation Information

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