Nitrochlorobenzene freezing point detection device

Abstract

The utility model discloses a nitrochlorobenzene freezing point detection device which comprises a base, and a test device, a power supply and control module and a freezing module are arranged on the base. A refrigerator is arranged in the freezing module and is used for providing cooling capacity for the test device; the power supply and control module comprises a power supply and a controller; the power supply is used for supplying power to the freezing module and the test device; the test device comprises a fixed table, a lifting driving device, a lifting table, a test container and a bath. The test container comprises a test bottle, a stirrer, a temperature sensor, a torque sensor, a test bottle cap and a dropwise adding meter. The controller judges whether the test sample reaches a freezing point or not according to the torque value of the stirring shaft, when the test sample reaches the freezing point, the controller stores the measured temperature of the temperature sensor, and the temperature is the freezing point temperature of the test sample. The nitrochlorobenzene freezing point detection device can replace manual work to automatically detect the nitrochlorobenzene freezing point, and is high in detection efficiency, high in detection precision and good in repeatability.

Description

TECHNICAL FIELD

[0001] The utility model relates to chemical detection technical field, concretely relates to a nitrochlorobenzene solidification point detection device. BACKGROUND

[0002] Nitrochlorobenzene is mainly used for the intermediate of dyes, pesticides, medicines, developing agent and rubber antioxidant, is also good high boiling point solvent and moderate organic oxidant, plays an important role in industrial production. Nitrochlorobenzene has broad market prospect. The preparation method of nitrochlorobenzene is: under the condition of waste acid, acid nitrochlorobenzene is generated by using chlorobenzene and mixed acid in annular nitrator, and after neutralization, washing and drying, crude nitrochlorobenzene is obtained, and after crystallization and rectification separation and purification, p-nitrochlorobenzene and o-nitrochlorobenzene finished products and by-product m-nitrochlorobenzene are obtained.

[0003] In the production and storage process, the freezing point of the compound can help to determine the appropriate operating temperature to avoid the solidification or melting of the material at improper temperature, and since the nitrochlorobenzene product obtained after separation and purification will be mixed with a small amount of impurities, it is necessary to detect the freezing point of the product in real time to ensure the product quality and stability in the production and transportation process.

[0004] The traditional detection method is:

[0005] (1) Principle: physically reduce the sample temperature, and when the solid phase begins to appear, the temperature is the freezing point.

[0006] (2) Instrument: 500mL beaker, magnetic stirrer, glass stirring rod and thermometer.

[0007] (3) Operation steps: firstly, add about 80mL of sample in the 500mL beaker, insert the stirring rod and thermometer, start to stir smoothly, no bubbles occur, start to appear crystallization, read the number when the temperature is relatively stable, and the result is retained after the decimal point.

[0008] The whole operation process of the traditional detection method of nitrochlorobenzene freezing point is manually carried out, which is time-consuming and laborious, and the efficiency is low, and the crystallization starting time is easy to miss and difficult to judge, and the detection precision is low. SUMMARY

[0009] To solve the above problems, the utility model provides a nitrochlorobenzene freezing point detection device.

[0010] The technical scheme adopted by the utility model is:

[0011] The nitrochlorobenzene solidification point detection device comprises a base, a test device, a power supply and control module, and a refrigeration module arranged on the base; a refrigerator is arranged in the refrigeration module, and the refrigerator is used for providing cold energy for the test device; the power supply and control module comprises a power supply and a controller, and the power supply is used for supplying power for the refrigeration module and the test device;

[0012] The test device comprises a fixing table, a lifting driving device, a lifting table, a test container and a bath, the bath is fixedly installed on the upper side of the fixing table, the upper end of the bath is open, the bath is filled with a cooling medium, and the cooling medium is connected with the refrigerator through a pipeline; the lifting table is located above the bath, the test container is installed on the lifting table, and the lifting table is driven to lift and descend by the lifting driving device; when the lifting table descends, the lower part of the test container can be immersed in the cooling medium in the bath;

[0013] The test container comprises a test bottle, a stirring motor, a stirrer, a temperature sensor, a torque sensor, a test bottle cap and a dropwise metering instrument, the test bottle is provided with a scale line, the test bottle cap is fixedly installed on the open end of the test bottle, the stirring motor of the stirrer is installed on the test bottle cap, a motor shaft vertically extends downwards and is connected with a stirring shaft through the torque sensor, the lower end of the stirring shaft extends into the test bottle and is connected with stirring blades, and the temperature sensor is inserted into the test bottle cap and has a contact head extending into the test bottle; the dropwise metering instrument is installed in a mounting hole of the test bottle cap and is used for dropping a test sample into the test bottle;

[0014] The refrigerator, the lifting machine, the stirring motor, the stirrer, the torque sensor and the temperature sensor are connected with the controller.

[0015] By adopting the technical scheme, the nitrochlorobenzene solidification point can be automatically detected instead of manual detection, and the detection precision and efficiency are greatly improved. The detection principle of the utility model is that when the test sample in the test bottle, namely, the sample, is dropped to a set volume; the test bottle is driven to descend into the bath by the lifting table, and the sample is completely immersed in the cooling medium; at this time, the stirring motor starts to work, the stirrer stirs the sample, and the controller detects the torque value of the stirring shaft detected by the torque sensor in real time; before the solidification point is reached, the sample is in a flowing state, the stirring force of the stirrer is small, and the torque value is low; when the sample begins to crystallize, the torque value of the stirring shaft suddenly increases; at this time, the controller stores the detection temperature value of the temperature sensor, and the temperature is the solidification point temperature of the sample.

[0016] Further, the utility model also comprises a connecting hose and a feed pump, the dropwise metering instrument is connected with the feed pump through the connecting hose, and the feed pump is connected with a nitrochlorobenzene storage tank.

[0017] By adopting the technical scheme, the feed pump and the connecting hose can be used to detect the solidification point of the material in the nitrochlorobenzene storage tank at any time, so as to ensure the stability and safety of the product in the storage process.

[0018] Further, the test container is three, three test containers are evenly distributed on the lifting platform in the circumferential direction, and the three test containers are respectively connected with three feed pumps through three connecting hoses, and the three feed pumps are respectively connected with the para-nitrochlorobenzene storage tank, the ortho-nitrochlorobenzene storage tank and the meta-nitrochlorobenzene storage tank.

[0019] By adopting the technical scheme, the freezing points of the three products can be detected respectively, and the work efficiency is high.

[0020] Further, a plurality of guide rods are installed on the fixing table, and the lifting platform is slidingly arranged on the guide rods, and the guide rods are uniformly distributed on the outer periphery of the bath.

[0021] By adopting the technical scheme, the lifting platform is lifted under the guidance of the guide rods, and the stability of lifting is improved.

[0022] Further, the lifting driving device comprises an elevator, the elevator is installed in the fixing table, and the telescopic rod of the elevator penetrates through the center hole of the bath upwards and is connected with the lifting platform.

[0023] By adopting the technical scheme, the lifting movement of the lifting platform can be realized, and the elevator is used as the driving force, so that the structure of the whole test device is compact.

[0024] Further, the lifting driving device comprises a driving cylinder, the driving cylinder is installed on the base through a support, and the cylinder piston rod is vertically downwardly extended and connected with the lifting platform.

[0025] By adopting the technical scheme, the lifting movement of the lifting platform can be realized, and the driving cylinder is used as the driving force, and the cylinder is installed outside the bath, so that the structure of the bath can be simplified.

[0026] Further, the test bottle is threadedly connected with the test bottle cap, so that the test bottle can be conveniently disassembled and cleaned.

[0027] Further, the test container is fixedly inserted on the lifting platform through the test bottle, and the lower part of the test bottle is extended from the bottom surface of the lifting platform, so that the test container can be conveniently disassembled and assembled.

[0028] The device has the advantages of compact structure, high reliability, and can replace manual detection of the freezing point of nitrochlorobenzene, has high detection efficiency, high detection precision and good repeatability. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 It is a structure diagram of a nitrochlorobenzene freezing point detection device of embodiment 1.

[0030] Figure 2 It is a top view of Figure 1 .

[0031] Figure 3 It is a structure diagram of a test container of embodiment 1.

[0032] Figure 4 A state diagram of the detection device of Example 1 when a sample is added dropwise.

[0033] Figure 5 A structural diagram of a nitrochlorobenzene freezing point detection device of Example 2. DETAILED DESCRIPTION

[0034] In order to make the purpose, technical scheme and advantages of the present application more clear, the technical scheme of the present application will be described clearly and completely below in combination with the drawings and a preferred embodiment. Example 1

[0035] Referring to Figures 1-4 The present embodiment provides a nitrochlorobenzene freezing point detection device, which comprises a base 1, a test device 10, a power supply and control module 20 and a refrigeration module 30.

[0036] The base 1 is used for mounting the test device 10, the power supply and control module 20 and the refrigeration module 30. In order to make the operation and connection simple, the test device 10 is mounted in the middle part of the base 1, and the power supply and control module 20 and the refrigeration module 30 are respectively mounted on the left and right sides of the test device 10. A refrigerator (not shown in the figure) is arranged in the refrigeration module 30, and the refrigerator is used for providing cold energy for the test device. The power supply and control module 20 comprises a power supply and a controller. The power supply is used for supplying power for the refrigeration module 30 and the test device 10. In the present embodiment, the power supply voltage is 220V±10%, and the power is 50Hz. The controller is used for controlling the automatic operation process of the sample device. In the present embodiment, the controller model is ISL81401.

[0037] The test device 10 comprises a fixed table 11, an elevator 16, a lifting table 15, a test container 14 and a bath 12.

[0038] The fixed table 11 is fixedly mounted on the base 1 by screws. The inside of the fixed table 11 is a hollow structure, and the center part of the upper side thereof is provided with a through hole for mounting the elevator. The bath 12 is fixedly mounted on the upper side of the fixed table 11 by embedding. Preferably, the bath 12 is a glass bath, which is convenient for observation. The upper end of the glass bath is open, and an equal-height glass tube is mounted in the middle part thereof. The lower end of the glass tube penetrates through the glass bath and is flush with the bottom surface of the glass bath. The space surrounded by the glass tube and the side wall of the glass bath is filled with cooling medium. The outer wall of the glass bath is provided with an inlet and an outlet (not shown in the figure) of the cooling medium. The cooling medium is connected with the refrigerator through a pipeline connected with the inlet and the outlet.

[0039] The outer edge of the upper side of the fixed table is vertically provided with eight guide rods 13, which are evenly distributed around the outer periphery of the bath 12. The lifting platform 15 is slidingly connected to the eight guide rods 13 and is located above the bath 12. Three test containers 14 are installed on the lifting platform 15. The elevator 16 is installed in the central cavity of the fixed table 11. The telescopic rod of the elevator is vertically upward and freely passes through the glass tube of the glass bath to connect with the lifting platform 15.

[0040] The test container 14 includes a test bottle 140, a stirrer, a temperature sensor 143, a torque sensor, a test bottle cap 144, and a dropwise metering instrument 145. The test bottle 140 is marked with a scale line, which can accurately control the addition amount of the test sample. Preferably, the test bottle 140 is a glass bottle, which is convenient for observation. Preferably, the test bottle cap 144 is a wooden cap, which is convenient for installing the stirring motor 141, the temperature sensor 143, and the dropwise metering instrument 145. The test bottle cap 144 is threadedly connected to the open end of the test bottle. The test container 14 is fixedly inserted into the lifting platform 15 through the test bottle 140. The lower part of the test bottle 140 extends from the bottom surface of the lifting platform. The test bottle cap 144 is clamped in the counterbore of the lifting platform 15. The stirrer includes a stirring motor 141, a stirring shaft, and stirring blades 142. The stirring motor 141 is fixedly installed on the test bottle cap 144. The motor shaft extends vertically downward to connect the stirring shaft through the torque sensor. The lower end of the stirring shaft extends into the test bottle 140 to connect the stirring blades 142.

[0041] The temperature sensor 143 is inserted into the test bottle cap 144, and the contact extends into the test bottle 410. In this embodiment, the temperature sensor is a PT100 type temperature probe.

[0042] The dropwise metering instrument 145 is installed in the mounting hole of the test bottle cap. The inlet end is used to connect a hose (not shown in the figure). The hose is connected to a nitrochlorobenzene storage tank through a feeding pump (not shown in the figure). Preferably, the hose is a PVC transparent steel wire hose. In this embodiment, the dropwise metering instrument is a DZDR-50 type.

[0043] In this embodiment, the three dropwise metering instruments of the three test containers 14 are respectively connected to three feeding pumps through three connecting hoses. The three feeding pumps are respectively connected to the p-nitrochlorobenzene storage tank, the o-nitrochlorobenzene storage tank, and the m-nitrochlorobenzene storage tank. Example 2

[0044] Referring to Figure 5 , this embodiment is basically the same as example 1, the difference is only that:

[0045] The lifting drive device includes a driving cylinder 17, which is installed on the base 1 through a support. The cylinder piston rod extends vertically downward to connect the lifting platform 15. The bath 12 has a complete structure.

[0046] The driving cylinder 17, the refrigerator, the lifting device 16, the stirring motor 141, the stirrer and the temperature sensor 143 are connected with the controller.

[0047] The method for using the rising detection device is:

[0048] Step 1) Start the refrigerator, and pre-cool the cooling medium in the bath 12 to a set temperature; the temperature of the test sample is usually 16-26℃, and the temperature of the cooling medium can be reduced to about 10℃.

[0049] Step 2) Make the test sample drop into the test bottle 140 through the dropwise meter 145, and control the adding amount of the test sample through the scale line on the test bottle; the adding amount of the test sample is 2ml.

[0050] Step 3) Start the lifting driving device, and make the lifting platform 15 drive the test container 14 to descend, and stop the lifting when the test sample in the test bottle 140 is completely immersed in the cooling medium in the bath; at the same time, start the stirring motor 141 to stir the test sample, and the temperature sensor 143 detects the temperature of the test sample.

[0051] Step 4) When the controller detects that the torque of the stirring shaft suddenly increases, it indicates that the test sample has reached the freezing point, at this time, the stirring motor 141 stops working, and the controller stores the detection result of the temperature sensor 143.

[0052] Step 5) Start the lifting driving device again, and make the lifting platform 15 and the test container 14 rise to the initial position.

[0053] The above method is used for measuring the freezing point of p-nitrochlorobenzene stored in a p-nitrochlorobenzene storage tank, and the detection result is shown in Table 1.

[0054]

[0055] From the detection result in Table 1, it can be known that the method has high detection precision and good repeatability.

[0056] The above only describes preferred embodiments of the present application, and it should be pointed out that, for ordinary skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements are also within the protection scope of the present application.

Claims

1. A nitrochlorobenzene freezing point detection device comprising a base (1), characterised in that, The base (1) is provided with a test device (10), a power supply and control module (20), and a refrigeration module (30); The refrigeration module (30) is provided with a refrigerator, which is used to provide cold energy for the test device; The power supply and control module (20) includes a power supply and a controller, and the power supply is used to supply power for the refrigeration module (30) and the test device (10); The test device (10) includes a fixed table (11), a lifting driving device, a lifting table (15), a test container (14), and a bath (12), the bath (12) is fixedly installed on the upper side of the fixed table (11), the upper end of the bath (12) is open, the bath (12) is filled with a cooling medium (2), and the cooling medium is connected with the refrigerator through a pipeline; the lifting table (15) is located above the bath (12), the test container (14) is installed on the lifting table (15), and the lifting table (15) is driven to lift by the lifting driving device; when the lifting table (15) is lowered, the lower part of the test container (14) can be immersed in the cooling medium in the bath (12); The test container (14) includes a test bottle (140), a stirrer, a temperature sensor (143), a torque sensor, a test bottle cap (144), and a dropwise metering instrument (145), the test bottle (140) is provided with a scale line, the test bottle cap (144) is fixedly installed on the open end of the test bottle (140), a stirring motor (141) of the stirrer is installed on the test bottle cap (144), a motor shaft vertically extends downward to connect a stirring shaft through the torque sensor, the stirring shaft extends into the test bottle (140) to connect stirring blades (142) at the lower end, the temperature sensor (143) is inserted into the test bottle cap (144), and a contact of the temperature sensor (143) extends into the test bottle (140); the dropwise metering instrument (145) is installed in a mounting hole of the test bottle cap (144) and is used to drop a test sample into the test bottle (140); The refrigerator, the lifting machine, the stirring motor (141), the stirrer, the torque sensor, and the temperature sensor (143) are connected with the controller.

2. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein The test device (10) further includes connecting hoses and feed pumps, the dropwise metering instrument (145) is connected with the feed pumps through the connecting hoses, and the feed pumps are connected with nitrochlorobenzene storage tanks.

3. A nitrochlorobenzene freeze point detection device as defined in claim 2, wherein The test container (14) has three test containers, and the three test containers are uniformly distributed on the lifting table (15) in a circumferential direction; the dropwise metering instruments of the three test containers are connected with the three feed pumps through three connecting hoses respectively, and the three feed pumps are connected with the para-nitrochlorobenzene storage tank, the ortho-nitrochlorobenzene storage tank, and the meta-nitrochlorobenzene storage tank respectively.

4. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein A plurality of guide rods (13) are further installed on the fixed table (11), the lifting table (15) is slidingly arranged on the guide rods, and the guide rods are uniformly distributed on the outer periphery of the bath (12).

5. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein The lifting driving device includes a lifting machine (16), the lifting machine (16) is installed inside the fixed table (11), and a telescopic rod of the lifting machine (16) penetrates through a center hole of the bath (12) upward to be connected with the lifting table (15).

6. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein The lifting driving device includes a driving cylinder, the driving cylinder is installed on the base (1) through a support, and a cylinder piston rod vertically extends downward to be connected with the lifting table (15).

7. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein The test bottle (140) is threadedly connected with the test bottle cap (144).

8. A nitrochlorobenzene freeze point detection device as defined in claim 1, wherein The test container (14) is fixedly inserted into the lifting table (15) through the test bottle (140), and the lower part of the test bottle (140) extends from the bottom surface of the lifting table (15).

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