CN216525002U

CN216525002U - Device for sampling of rectifying tower

Info

Publication number: CN216525002U
Application number: CN202122682191.2U
Authority: CN
Inventors: 张亮; 周志祥; 吴小峰; 方满堂; 蒋权; 王志国
Original assignee: Huangshi Fuertai Pharmaceutical Tech Co ltd
Current assignee: Huangshi Fuertai Pharmaceutical Tech Co ltd
Priority date: 2021-11-04
Filing date: 2021-11-04
Publication date: 2022-05-13
Anticipated expiration: 2031-11-04

Abstract

The utility model discloses a device for sampling a rectifying tower, which comprises a lifting platform, a vacuum pump and a bottom plate, wherein the top of the lifting platform is connected with a heating pot, the top of the heating pot is provided with a tower kettle, the top of the tower kettle is fixedly communicated with a tower section, the top of the tower section is fixedly connected with a tower head, the tower head comprises a steam pipeline and a return pipeline, the top between the steam pipeline and the return pipeline and the bottom between the steam pipeline and the return pipeline are respectively and fixedly communicated with a connecting pipe and a U-shaped return pipe, the U-shaped groove of the U-shaped return pipe is fixedly communicated with a sampling piston, and the bottom of the return pipeline is fixedly communicated with a receiving tank; the sampling operation is simple, convenient and quick; the defects that the vacuum needs to be frequently unloaded and the stability of a rectification system is damaged during sampling are overcome; the sampling point that needs to collect can be found more fast, the quality and the yield of the product that need collect are improved, improve rectification efficiency.

Description

Device for sampling of rectifying tower

Technical Field

The utility model relates to the field of chemical equipment, in particular to a device for sampling a rectifying tower.

Background

With the upgrading of industries, the requirements of various industries on the product quality are continuously improved, and the application of a rectification method to improve the product quality is an important economic means which cannot be replaced by other purification methods. The rectifying tower is a tower type vapor-liquid contact device for rectification. By utilizing the property that each component in the mixture has different volatility, namely the vapor pressure of each component is different at the same temperature, the light component (low-boiling-point substance) in the liquid phase is transferred into the gas phase, and the heavy component (high-boiling-point substance) in the gas phase is transferred into the liquid phase, thereby realizing the purpose of separation. The glass rectification device in the laboratory is a necessary device for performing product development experiments, purification and refining substances in the departments of fine chemical industry, daily chemical industry, light chemical industry, pharmaceutical industry, petroleum refining, agriculture and forestry chemical industry and the like, and is also important experimental equipment for scientific research and teaching of colleges and universities. In the rectification and purification process of product development, in order to ensure the purity of the rectification product, the middle control sampling operation is required to be frequently carried out. The quality of the product is continuously determined by the central control sampling, the yield of the product can be improved, and the convenient and fast sampling mode is more beneficial to optimizing the rectification parameters. Due to limitation, the laboratory glass rectifying tower needs to release pressure in the sampling process, or partially release the pressure, or is monitored by methods of detecting products, monitoring parameters and the like. Most of the operations require vacuum rectification, the rectification temperature is high, the vacuum requirement is high, and once the pressure is relieved, the operation needs a long time for stabilization. Some products sensitive to air humidity and oxygen are damaged and decomposed even in the pressure relief process. And the control by various parameters greatly possibly causes low product purity or great waste due to the complex actual operation condition of rectification. The central control sampling brings about a certain trouble to the rectification operation but is indispensable.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a device for sampling a rectifying tower, which aims to solve the problem that the laboratory glass rectifying tower provided by the background art needs pressure relief or partial pressure relief in the sampling process due to limitation, or is monitored by methods of detecting products, monitoring parameters and the like. Most of the operations require vacuum rectification, the rectification temperature is high, the vacuum requirement is high, and once the pressure is relieved, the operation needs a long time for stabilization. Some products sensitive to air humidity and oxygen are damaged and decomposed even in the pressure relief process. And the control by various parameters greatly causes the problems of low product purity or great waste due to the complex actual operation condition of rectification.

In order to achieve the purpose, the utility model provides the following technical scheme: a device for sampling a rectifying tower comprises a lifting platform, a vacuum pump and a bottom plate, wherein the top of the lifting platform is connected with a heating pot, the top of the heating pot is provided with a tower kettle, the top of the tower kettle is fixedly communicated with a tower section, the top of the tower section is fixedly connected with a tower head, the tower head comprises a steam pipeline and a return pipeline, the top between the steam pipeline and the return pipeline and the bottom between the steam pipeline and the return pipeline are respectively and fixedly communicated with a connecting pipe and a U-shaped return pipe, a U-shaped groove of the U-shaped return pipe is fixedly communicated with a sampling piston, the bottom of the return pipeline is fixedly communicated with a receiving tank, one side of the receiving tank is communicated with a first pipeline, a receiving tank vent is arranged at the joint of the receiving tank and the first pipeline, the top of the return pipeline is communicated with a second pipeline communicated with the first pipeline, one end of the second pipeline, which is far away from the return pipeline, is communicated with a buffer tank, the buffer tank is communicated with a third pipeline and a fourth pipeline, a buffer tank vent is arranged on the third pipeline, one end, away from the buffer tank, of the fourth pipeline is communicated with an input port of the vacuum pump, and the buffer tank and the vacuum pump are both installed at the top of the bottom plate.

Preferably, thermometers are arranged on the tower kettle, the tower section, the tower head and the buffer tank.

Preferably, a piston tail groove is formed in the periphery of one end of the sampling piston, a connecting groove is formed in the middle of the other end of the sampling piston, a rotating handle is fixedly connected with the connecting groove, a sample liquid containing cavity is formed in the sampling piston, and a one-way port communicated with the sample liquid containing cavity is formed in the surface of the sampling piston.

Preferably, the connection part of the return pipeline and the receiving tank and the bottom of the receiving tank are both provided with a switch piston.

Preferably, the inside of backflow pipeline is equipped with the condenser and is located the collection funnel of condenser below, the U type back flow just passes backflow pipeline to the one end of backflow pipeline and extends to under the collection funnel.

Preferably, the surface of the return pipeline is provided with an electromagnet, the collection funnel is connected with a metal valve core in a sliding manner, and the electromagnet and the metal valve core are arranged correspondingly.

Preferably, a three-way valve is installed at the joint of the first pipeline and the second pipeline, and one-way valves are installed in the middle of the third pipeline and the middle of the fourth pipeline.

Compared with the prior art, the utility model has the beneficial effects that: the structure is simple; the sampling operation is simple, convenient and quick; the defects that the stability of a rectification system is damaged due to frequent vacuum unloading during sampling are overcome; the sampling point that needs to collect can be found more fast, the quality and the yield of the product that need collect are improved, improve rectification efficiency.

Drawings

FIG. 1 is a schematic structural view of the present invention;

fig. 2 is a schematic structural diagram of a sampling piston according to the present invention.

In the figure: 1. a tower kettle; 2. tower sections; 3. a condenser; 4. a tower head; 5. a receiving tank; 6. an electromagnet; 7. a vacuum pump; 8. a receiving tank vent; 9. a buffer tank vent; 10. heating and cooking; 11. a lifting platform; 12. a sampling piston; 13. a thermometer; 14. connecting grooves; 15. rotating the handle; 16. a piston tail groove; 17. a sample loading cavity; 18. a one-way port; 19. a buffer tank; 20. a base plate.

Detailed Description

The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.

Referring to fig. 1-2, the utility model provides a device for sampling a rectifying tower, comprising a lifting platform 11, a vacuum pump 7 and a bottom plate 20, wherein the top of the lifting platform 11 is connected with a heating pot 10, the top of the heating pot 10 is provided with a tower kettle 1, the top of the tower kettle 1 is fixedly communicated with a tower section 2, the top of the tower section 2 is fixedly connected with a tower head 4, the tower head 4 is a common rectifying head in the market, the tower head 4 comprises a steam pipeline and a return pipeline, the top between the steam pipeline and the return pipeline and the bottom between the steam pipeline and the return pipeline are respectively fixedly communicated with a connecting pipe and a U-shaped return pipe, a U-shaped groove of the U-shaped return pipe is fixedly communicated with a sampling piston 12, the bottom of the return pipeline is fixedly communicated with a receiving tank 5, one side of the receiving tank 5 is communicated with a first pipeline, the connecting part of the receiving tank 5 and the first pipeline is provided with a receiving tank vent 8, the top of the return pipeline is communicated with a second pipeline communicated with the first pipeline, the one end intercommunication that return line was kept away from to the second pipeline has buffer tank 19, and the intercommunication has third pipeline and fourth pipeline on the buffer tank 19, is equipped with buffer tank drain 9 on the third pipeline, and the one end that buffer tank 19 was kept away from to the fourth pipeline communicates with the input port of vacuum pump 7, and buffer tank 19 and vacuum pump 7 are all installed in the top of bottom plate 20.

The thermometers 13 are respectively arranged on the tower bottom 1, the tower section 2, the tower head 4 and the buffer tank 19, and the thermometers 13 are used for sensing the temperatures in the tower bottom 1, the tower section 2, the tower head 4 and the buffer tank 19.

A piston tail groove 16 is arranged on the periphery of one end of a sampling piston 12, a connecting groove 14 is arranged in the middle of the other end of the sampling piston 12, the connecting groove 14 is fixedly connected with a rotating handle 15, a sample liquid containing cavity 17 is arranged inside the sampling piston 12, a one-way port 18 communicated with the sample liquid containing cavity 17 is arranged on the surface of the sampling piston 12, the one-way port 18 is kept downward, a rubber band is used for binding and fixing the connecting groove 14 of the piston and the piston tail groove 16, temperature rise rectification can be carried out, after liquid discharge is stable, when sampling is needed, the one-way port 18 is vertically upward rotated by 180 degrees through the rotating handle 15, the material at the U-shaped groove of a U-shaped return pipe flows into the sample liquid containing cavity 17 for a short time, a 1.5ml centrifugal pipe is used below the sampling piston 12 for receiving the material, then the rotating handle 15 is rotated by 180 degrees, the one-way port 18 is vertically downward, the material flows out to the 1.5ml centrifugal pipe through the one-way port 18, and (5) finishing sampling operation, and detecting the liquid sample by using a gas chromatograph.

Electromagnet 6 corresponds the setting with the metal case, and return line's inside is equipped with condenser 3 and is located the collection funnel of condenser 3 below, and return line all installs the switch piston with the junction of receiving jar 5 and the bottom of receiving jar 5, and return line's surface is equipped with electromagnet 6, and sliding connection has the metal case on the collection funnel, and U type back flow just passes return line to return line's one end and extends to under the collection funnel.

The junction of first pipeline and second pipeline installs the three-way valve, opens through first pipeline of three-way valve control or second pipeline, and the check valve is all installed at the middle part of third pipeline and the middle part of fourth pipeline, opens or is closed through check valve control third pipeline and fourth pipeline to open or closed buffer tank drain 9 and vacuum pump 7.

When the embodiment of the application is used: keeping the one-way port 18 downward, binding the piston tail groove 16 of the sampling piston 12 with the piston tail groove 16 by using a rubber band, thereby fixing the sampling piston 12, adding 2/3-volume crude chloromethyl ethyl carbonate into the tower kettle 1, adjusting the lifting platform 11 to fix the tower kettle 1, starting cooling water of the condenser 3, closing the vent 9 of the buffer tank, starting the vacuum pump 7, adjusting the heating pot 10 to be 70 ℃, gradually increasing the temperature of the tower section 2 to 60 ℃ along with the time increase, gradually increasing the temperature of the tower head 4 to 30 ℃, adjusting the electromagnet 5, opening a metal valve core on the collecting funnel, collecting the previous fraction into the receiving tank 5, sampling when the temperature of the tower head 4 is gradually increased to 52 ℃, rotating the handle 15 by 180 ℃ to enable the one-way port 18 to vertically face upward, slightly waiting for a moment, enabling the material at the U-shaped groove of the U-shaped return pipe to flow into the sample liquid-containing cavity 17, using a 1.5ml centrifugal tube below a sampling piston 12 to receive materials, rotating a handle 15 for 180 degrees to enable a one-way port 18 to be vertically downward, enabling the materials to flow out of the 1.5ml centrifugal tube from the one-way port 18, completing sampling operation, detecting a liquid sample by using a gas chromatograph until the content reaches 99%, discharging the materials in a receiving tank 5, starting to receive a finished product, carrying out sampling operation at middle interval time, adjusting the temperature of a heating pot 10 according to the condensation flow of a condenser 3, carrying out sampling operation when the temperature of a tower head 4 is gradually increased to 63 ℃, discharging the product of the receiving tank 5 when the content of single impurities is higher than 0.6% and lower than 99%, starting to receive the fraction, adjusting an electromagnet 6, rapidly extracting the fraction, closing the heating pot 10 after no fraction, closing a vacuum pump 7, closing the condenser 3, and stopping the experiment.

Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the utility model can be made, and equivalents and modifications of some features of the utility model can be made without departing from the spirit and scope of the utility model.

Claims

1. A device for rectifying column sampling, includes elevating platform (11), vacuum pump (7) and bottom plate (20), its characterized in that: the top of the lifting platform (11) is connected with a heating pot (10), the top of the heating pot (10) is provided with a tower kettle (1), the top of the tower kettle (1) is fixedly communicated with a tower section (2), the top of the tower section (2) is fixedly connected with a tower head (4), the tower head (4) comprises a steam pipeline and a return pipeline, the top between the steam pipeline and the return pipeline and the bottom between the steam pipeline and the return pipeline are respectively and fixedly communicated with a connecting pipe and a U-shaped return pipe, a U-shaped groove of the U-shaped return pipe is fixedly communicated with a sampling piston (12), the bottom of the return pipeline is fixedly communicated with a receiving tank (5), one side of the receiving tank (5) is communicated with a first pipeline, a receiving tank emptying port (8) is arranged at the joint of the receiving tank (5) and the first pipeline, and the top of the return pipeline is communicated with a second pipeline communicated with the first pipeline, the one end intercommunication that backflow pipeline was kept away from to the second pipeline has buffer tank (19), the intercommunication has third pipeline and fourth pipeline on buffer tank (19), is equipped with buffer tank drain (9) on the third pipeline, and the one end that buffer tank (19) were kept away from to the fourth pipeline communicates with the input port of vacuum pump (7), the top in bottom plate (20) is all installed in buffer tank (19) and vacuum pump (7).

2. An apparatus for sampling a rectification column in accordance with claim 1, wherein: thermometers (13) are arranged on the tower kettle (1), the tower section (2), the tower head (4) and the buffer tank (19).

3. An apparatus for sampling a rectification column in accordance with claim 1, wherein: piston afterbody groove (16) have been seted up to the periphery of sample piston (12) one end, connecting groove (14) have been seted up at the middle part of sample piston (12) other end, connecting groove (14) fixedly connected with twist grip (15), sample dress liquid chamber (17) have been seted up to the inside of sample piston (12), one-way mouth (18) with sample dress liquid chamber (17) intercommunication are seted up on the surface of sample piston (12).

4. An apparatus for sampling a rectification column in accordance with claim 1, wherein: switch pistons are arranged at the joint of the return pipeline and the receiving tank (5) and at the bottom of the receiving tank (5).

5. An apparatus for sampling a rectification column in accordance with claim 1, wherein: the inside of return line is equipped with condenser (3) and is located the collection funnel of condenser (3) below, U type back flow just passes the return line to the one end of return line and extends to under the collection funnel.

6. An apparatus for sampling a rectification column in accordance with claim 5, wherein: the surface of the backflow pipeline is provided with an electromagnet (6), the collection funnel is connected with a metal valve core in a sliding mode, and the electromagnet (6) is arranged corresponding to the metal valve core.

7. An apparatus for sampling a rectification column in accordance with claim 1, wherein: a three-way valve is installed at the joint of the first pipeline and the second pipeline, and one-way valves are installed in the middle of the third pipeline and the middle of the fourth pipeline.