CN210665485U

CN210665485U - Sampling device of rectifying tower in phenylethylamine production

Info

Publication number: CN210665485U
Application number: CN201921351104.1U
Authority: CN
Inventors: 韩兵; 李晓平
Original assignee: Haicheng Leach Carbon Materials Co Ltd
Current assignee: Haicheng Leach Carbon Materials Co Ltd
Priority date: 2019-08-20
Filing date: 2019-08-20
Publication date: 2020-06-02
Anticipated expiration: 2029-08-20

Abstract

The utility model belongs to the technical field of chemical production, in particular to a sampling device of a rectifying tower in phenylethylamine production, which is characterized by comprising a sampling tank, a vacuum loop valve, a nitrogen pressurizing valve, an analysis valve and a recovery valve, wherein one end of the sampling tank is connected with a sampling port of the rectifying tower through a main valve and a quick self-sealing joint in sequence, the vacuum loop valve is connected with a vacuum pump, and the nitrogen pressurizing valve is connected with a nitrogen tank; the analysis valve is connected with the spectrophotometry analyzer, the recovery valve is communicated with a waste liquid recovery tank, and the waste liquid recovery tank is communicated with the bottom of the rectifying tower through a waste liquid recovery pump. Compared with the prior art, the beneficial effects of the utility model are as follows: 1) the quick self-sealing joint can be quickly separated from the rectifying tower, and the maintenance of the device is convenient. 2) The in-process sample liquid of sample does not contact with the external world, has effectively prevented impurity invasion sample liquid, guarantees the reliability of sample liquid analysis. 3) Set up artifical manual sample connection, guarantee the normal sample under the unconventional condition.

Description

Sampling device of rectifying tower in phenylethylamine production

Technical Field

The utility model belongs to the technical field of chemical production, especially, relate to a sampling device of rectifying column in phenylethylamine production.

Background

The rectifying tower is a separation device commonly used in the chemical field, also called as a distillation device, and is a vapor-liquid contact type separation and purification device, when the separation is carried out, vapor enters from the bottom of the rectifying tower, the evaporated gas phase is in countercurrent contact with descending liquid, in the process of two-phase contact, volatile (low boiling point) components in the descending liquid are continuously transferred to the gas phase, nonvolatile (high boiling point) components in the gas phase are continuously transferred to the descending liquid, the concentration of the volatile components is higher as the gas phase is closer to the top of the tower, and the volatile components are more enriched as the descending liquid is closer to the bottom of the rectifying tower, so that the purpose of component separation is achieved.

Rectification in the production process of phenylethylamine is one of the most critical processes for the final high-purity extraction, and sampling is a critical link for detecting whether the produced product meets the requirements of the production process. The phenethylamine is an aromatic amine, is a colorless liquid at room temperature, but has fishy smell which can volatilize into the air, and if the sampling process is not sealed, the production environment can be polluted, and the body of an operator can be damaged. In addition, the sampling process may also cause the sample to be interfered by the external environment, and if impurities are mixed into the sample in the sampling process, the detection result of the test sample may also have a certain deviation.

The Chinese utility model with the patent application number of 201520829382.9 discloses an organic phosphine negative pressure rectification sampling device, which comprises a sampling tube, a receiving tank, a nitrogen communicating tube and a vacuum pump connecting tube, wherein the upper end of the sampling tube is communicated with the side surface of an organic phosphine rectification outlet tube, and the bottom end of the sampling tube is movably and hermetically connected with the receiving tank; a stop valve is arranged at one end of the sampling pipe close to the organic phosphine rectification outlet pipe; the part of the sampling tube below the stop valve is connected with one end of a nitrogen communicating tube, and the other end of the nitrogen communicating tube is used for connecting a nitrogen tank; the part of the sampling tube below the stop valve is also connected with one end of a vacuum pump connecting pipe, and the other end of the vacuum pump connecting pipe is used for connecting a vacuum pump; the nitrogen gas communicating pipe and the vacuum pump connecting pipe are respectively provided with a gas valve and a vacuum valve. This device simple structure, convenient operation can take a sample under negative pressure state, can dismantle cleanly to the organic phosphine sample of protection sample jar is not by the oxidation. Sampling device has that the sampling rate is fast among this literature, and the leakproofness is good, can avoid receiving the advantage of external environment interference, and its shortcoming can not the analysis on the spot, can only send the sample to the laboratory and detect, and the inefficiency ratio is lower, does not have the link of collecting the sample waste liquid in addition, has not avoided can not causing the pollution to the environment.

Disclosure of Invention

The utility model aims at providing a sampling device of rectifying column in phenylethylamine production, overcome the not enough of prior art, can realize taking a sample from the rectifying column fast, complementary with artifical manual sample, degree of automation is high, can keep whole sample process to go on under sealed condition, avoid compound to leak the pollution to the production environment, cause harm to operating personnel health, in addition, still can avoid the sample to receive external environment's interference, it is more accurate to make chemical examination analysis result, and then correctly guide production.

In order to achieve the above object, the utility model discloses a following technical scheme realizes:

a sampling device of a rectifying tower in phenylethylamine production is characterized by comprising a sampling tank, a vacuum loop valve, a nitrogen pressurizing valve, an analysis valve and a recovery valve, wherein one end of the sampling tank is sequentially connected with a sampling port of the rectifying tower through a main valve and a quick self-sealing joint, the other end of the sampling tank is respectively connected with one end of the vacuum loop valve and one end of the nitrogen pressurizing valve, the other end of the vacuum loop valve is connected with a vacuum pump through a first flexible connecting pipe, and the other end of the nitrogen pressurizing valve is connected with a nitrogen tank; one end of the sampling tank is connected with one end of an analysis valve, the other end of the analysis valve is connected with an A port of a four-way valve, a B port of the four-way valve is connected with a spectrophotometry analyzer through a second flexible connecting pipe, a C port of the four-way valve is connected with one end of a recovery valve, and a D port of the four-way valve is connected with a manual sampling rubber plug; the other end of the recovery valve is communicated with a waste liquid recovery tank, and the waste liquid recovery tank is communicated with the bottom of the rectifying tower through a waste liquid recovery pump.

At least one of the vacuum loop valve, the nitrogen pressurization valve, the analysis valve and the recovery valve is an electric ball valve, an electric gate valve or a pneumatic butterfly valve.

And a pressure gauge and/or a pressure reducing valve are/is arranged on a pipeline between the other end of the sampling tank and one end of the vacuum loop valve.

And a liquid level sensor is arranged on the sampling tank.

The spectrophotometry analyzer is communicated with a background computer through an RS232 protocol, and the background computer is connected with a terminal display.

The quick self-sealing joint is an SP-A quick joint of ｃA Nidong tool.

The waste liquid recovery pump is a pipeline type centrifugal pump.

The spectrophotometry analyzer is a 756PC series digital display ultraviolet visible spectrophotometry.

Compared with the prior art, the beneficial effects of the utility model are as follows: 1) the quick self-sealing joint can be quickly separated from the rectifying tower, and the maintenance of the sampling device is convenient. 2) The sample liquid is sucked by negative pressure, and the sample liquid is not contacted with the outside in the sampling process, so that external impurities are effectively prevented from invading the sample liquid, and the reliability of sample liquid analysis is ensured. 3) The device uses the hose coupling to keep apart the vacuum pump, has reduced the influence of vibration to system stability. 4) And the sample liquid is pushed and pressed to the ultraviolet visible spectrophotometer by adopting nitrogen, so that the sample liquid is effectively isolated from contacting the outside, and the sample liquid is further prevented from being polluted. 5) Set up artifical manual sample connection, guarantee the normal sample under the unconventional condition, the flexibility is strong. 6) The residual sample liquid in the sample tank at the end can be automatically emptied after sampling, and the effectiveness of the sample liquid sampled next time is fully ensured. 7) Waste liquid accessible waste liquid recovery pump is retrieved to the rectifier bottom, realizes that whole process does not have waste liquid and discharges, realizes whole sampling device's economic nature and environmental protection. 8) The ultraviolet-visible spectrophotometer can be communicated with an industrial computer, and can be used for storing and counting sample data analyzed each time, so that the product data can be conveniently analyzed in the later period.

Drawings

FIG. 1 is a schematic view of the structure of the sampling device of the rectification column in the production of phenylethylamine according to the present invention.

Fig. 2 is a schematic structural view of the manual sampling rubber plug of the present invention.

In the figure: 1-a main valve, 2-a quick self-sealing joint, 31-a vacuum loop valve, 32-a nitrogen pressurization valve, 33-an analysis valve, 34-a recovery valve, 4-a sampling tank, 5-a liquid level sensor, 6-a pressure gauge, 7-a pressure reducing valve, 8-a first flexible connecting pipe, 9-a vacuum pump, 10-a nitrogen tank, 11-a manual sampling rubber plug, 12-an ultraviolet visible spectrophotometer, 13-a waste liquid recovery tank, 14-a waste liquid recovery pump, 15-an industrial computer, 16-a terminal display, 17-a rectifying tower, 18-a second flexible connecting pipe and 19-a four-way valve.

Detailed Description

The following embodiments are further described in the following:

in the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.

See fig. 1, fig. 2, is the utility model relates to a sampling device embodiment schematic structure diagram of rectifying column in phenylethylamine production, the one end of sample jar 4 is connected with rectifying column 17's sample connection through main valve 1, quick valve connector 2 in proper order, is equipped with level sensor 5 on the sample jar 4.

The other end of the sampling tank 4 is respectively connected with one end of a vacuum loop valve 31 and one end of a nitrogen pressurization valve 32, a pressure gauge 6 and a pressure reducing valve 7 are arranged on a pipeline between the other end of the sampling tank 4 and one end of the vacuum loop valve 31, the other end of the vacuum loop valve 31 is connected with a vacuum pump 9 through a first flexible connecting pipe 8, and the other end of the nitrogen pressurization valve 32 is connected with a nitrogen tank 10; one end of the sampling tank 4 is also connected with one end of an analysis valve 33, the other end of the analysis valve 33 is connected with an A port of a four-way valve 19, a B port of the four-way valve 19 is connected with an ultraviolet-visible spectrophotometer 12 through a second flexible connecting pipe 18, a C port of the four-way valve 19 is connected with one end of a recovery valve 34, a D port of the four-way valve 19 is connected with a manual sampling rubber plug 11, and the manual sampling rubber plug 11 comprises a sealing rubber sheet 110 and a D port threaded cover 111 for fixing the sealing rubber sheet to the four-way valve 19; the other end of the recovery valve 34 is communicated with the waste liquid recovery tank 13, and the waste liquid recovery tank 13 is communicated with the bottom of the rectifying tower 17 through the waste liquid recovery pump 14. The waste liquid recovery pump 14 is a centrifugal pump of the piping type.

The quick self-sealing joint 2 is ｃA Nidong worker SP-A quick joint which is generally used as ｃA transition joint for connecting ｃA rubber pipe and ｃA pipeline, two sets of opposite valves are arranged in one set of joint, and ｃA fluid passage can be connected and disconnected by rotating the joint by hands.

In the embodiment, the vacuum loop valve 31, the nitrogen pressurizing valve 32, the analyzing valve 33 and the recovery valve 34 are all Q941F-16PDN15 type electric ball valves which can be opened and closed under remote control, so that remote control sampling is realized.

The ultraviolet-visible spectrophotometer 12 is a 756PC series digital display ultraviolet-visible spectrophotometer manufactured by shanghai, and analysis data thereof is communicated with a background computer through an RS232 protocol and displayed on a terminal display of the background computer. The ultraviolet-visible spectrophotometer is an analyzer based on ultraviolet-visible spectrophotometry principle and utilizing the radiation absorption of substance molecules to the ultraviolet-visible spectrum region for analysis. Experiments prove that the hydrogen bond strength generated by different polar solvents is different, and the ultraviolet spectrum can be used for judging the hydrogen bond strength of the compound in different solvents so as to determine which solvent is selected.

The utility model discloses a theory of operation is: the rectified phenylethylamine separated from the rectifying tower 17 enters a sampling tank 4 through a quick self-sealing joint 2 and a main valve 1 on a pipeline. And starting a vacuum pump 9 to slowly flow the sample liquid into the sampling tank 4 through a first flexible connecting pipe 8, a pressure reducing valve 7 and a pressure gauge 6. When the sample liquid in the sampling tank 4 reaches the preset liquid level, the liquid level sensor 5 is triggered, and the vacuum pump 9 stops working. The sample can be selected from a manual sampling rubber plug 11 or sent to an ultraviolet visible spectrophotometer 12 for automatic analysis, and the two processes are carried out. After the automatic analysis process is selected, the nitrogen pressurization valve 32 and the analysis valve 33 are opened, and the sample liquid is pushed into the ultraviolet-visible spectrophotometer 12 by the nitrogen pressure. The data analyzed by the ultraviolet-visible spectrophotometer 12 is transmitted to the industrial computer 15 for recording and saving through an RS232 protocol. The recovery valve 34 is opened, the waste liquid in the sampling tank 4 is discharged to the waste liquid recovery tank 13, the waste liquid recovery pump 14 is opened, the waste liquid in the waste liquid recovery tank 13 is recovered to the bottom of the rectifying tower 1, and the sampling process is finished.

The above-mentioned embodiments are only specific examples selected for the purpose of illustrating the objects, technical solutions and advantages of the present invention in detail, but should not limit the scope of the present invention, and all modifications, equivalent substitutions and improvements made without departing from the spirit and principles of the present invention should fall within the scope of the present invention.

Claims

1. A sampling device of a rectifying tower in phenylethylamine production is characterized by comprising a sampling tank, a vacuum loop valve, a nitrogen pressurizing valve, an analysis valve and a recovery valve, wherein one end of the sampling tank is sequentially connected with a sampling port of the rectifying tower through a main valve and a quick self-sealing joint, the other end of the sampling tank is respectively connected with one end of the vacuum loop valve and one end of the nitrogen pressurizing valve, the other end of the vacuum loop valve is connected with a vacuum pump through a first flexible connecting pipe, and the other end of the nitrogen pressurizing valve is connected with a nitrogen tank; one end of the sampling tank is connected with one end of an analysis valve, the other end of the analysis valve is connected with an A port of a four-way valve, a B port of the four-way valve is connected with a spectrophotometry analyzer through a second flexible connecting pipe, a C port of the four-way valve is connected with one end of a recovery valve, and a D port of the four-way valve is connected with a manual sampling rubber plug; the other end of the recovery valve is communicated with a waste liquid recovery tank, and the waste liquid recovery tank is communicated with the bottom of the rectifying tower through a waste liquid recovery pump.

2. The sampling device of the rectification column in the production of phenylethylamine according to claim 1, wherein at least one of the vacuum loop valve, the nitrogen pressurization valve, the analysis valve and the recovery valve is an electric ball valve, an electric gate valve or a pneumatic butterfly valve.

3. The sampling device of the rectification column in the production of phenylethylamine according to claim 1, wherein a pressure gauge and/or a pressure reducing valve is arranged on a pipeline between the other end of the sampling tank and one end of the vacuum loop valve.

4. The sampling device of the rectification column in the production of phenylethylamine according to claim 1, wherein a liquid level sensor is arranged on the sampling tank.

5. The sampling device of the rectification tower in the production of phenethylamine according to claim 1, wherein the spectrophotometric analyzer is communicated with a background computer through an RS232 protocol, and the background computer is connected with a terminal display.

6. The sampling device of the rectifying tower in the production of phenethylamine according to claim 1, wherein the quick self-sealing joint is ｃA Nidoku SP-A quick joint.

7. The sampling device of the rectification column in the production of phenethylamine according to claim 1, wherein the waste liquid recovery pump is a pipe centrifugal pump.

8. The sampling device of the rectification column in the production of phenethylamine according to claim 1, wherein the spectrophotometric analyzer is a 756PC series digital display ultraviolet visible spectrophotometric instrument.