CN217819522U

CN217819522U - Vacuum liquid sampler

Info

Publication number: CN217819522U
Application number: CN202221264135.5U
Authority: CN
Inventors: 林如平; 杨建明; 王荣杰
Original assignee: Zhejiang Huahai Pharmaceutical Co Ltd; Zhejiang Huahai Licheng Pharmaceutical Co Ltd
Current assignee: Zhejiang Huahai Pharmaceutical Co Ltd; Zhejiang Huahai Licheng Pharmaceutical Co Ltd
Priority date: 2022-05-24
Filing date: 2022-05-24
Publication date: 2022-11-15
Anticipated expiration: 2032-05-24

Abstract

The utility model discloses a vacuum liquid sampler, which comprises a sample cavity, a sampling tube, a vacuum tube, a cleaning tube, a micro-pressure nitrogen tube and a side tube, wherein the vacuum tube, the cleaning tube and the micro-pressure nitrogen tube are connected above the sample cavity, and the upper part of the vacuum tube, the cleaning tube and the micro-pressure nitrogen tube are respectively connected with a vacuum valve, a cleaning valve and a micro-pressure nitrogen valve; the sampling tube is connected below the sample chamber, a first feed liquid valve is arranged in the middle of the sampling tube, and a tube opening connecting flange is arranged at the lower part of the sampling tube; the side tube is connected between the sample chamber and the sampling tube, a sampling bottle is arranged below the middle section of the side tube, and the tail end of the side tube is provided with a back flushing nitrogen valve; and a second feed liquid valve is arranged on the front section of the side pipe or on the pipeline of the sampling pipe between the sample chamber and the side pipe. The utility model discloses a vacuum principle takes out the sample cavity with liquid material from reation kettle, has reduced the pollution risk.

Description

Vacuum liquid sampler

Technical Field

The utility model belongs to the technical field of sampling device, more specifically relates to a vacuum liquid sampler who takes a sample is carried out to the feed liquid of airtight system.

Background

In pharmaceutical and chemical enterprises, the sampling of feed liquid is an important part of quality management, and the authenticity of the sample directly reflects the properties of materials. The existing sampling technology comprises modes of on-line pumping circulation sampling, vacuum material suction sampling, open sampling and the like.

Open sampling requires opening the reaction vessel, which may affect the reaction process in the reaction vessel and introduce impurities. The circulation sampling needs to be provided with a medium circulation outlet pipeline and an additional vent hole, so that the silting of a sampling medium is easily caused, and after the sampling is finished, residual liquid is easily generated in a sampling pipe, so that the waste of the sampling medium is easily caused. The existing sampler for vacuum material suction sampling comprises a sampling cavity, wherein the sampling cavity is communicated with a reaction kettle through a pipeline, a valve is arranged on the pipeline, and the valve is closed after liquid enters the sampling cavity. During the sampling process, feed liquid may remain in a sampling cavity or a sampling pipeline, and the sampling accuracy is affected.

SUMMERY OF THE UTILITY MODEL

The to-be-solved technical problem of the utility model is to avoid the uncovered sample and/or the feed liquid remaining in the sampler when taking a sample to reation kettle.

In order to solve the technical problem, the utility model provides a vacuum liquid sampler, which comprises a sample chamber, a sampling tube, a vacuum tube, a cleaning tube, a micro-pressure nitrogen tube and a side tube;

the vacuum tube, the cleaning tube and the micro-pressure nitrogen tube are connected above the sample chamber, and the upper parts of the vacuum tube, the cleaning tube and the micro-pressure nitrogen tube are respectively connected with a vacuum valve, a cleaning valve and a micro-pressure nitrogen valve;

the sampling tube is connected below the sample chamber, a first feed liquid valve is arranged in the middle of the sampling tube, and a tube opening connecting flange is arranged at the lower part of the sampling tube; the side tube is connected between the sample chamber and the sampling tube, a sampling bottle is arranged below the middle section of the side tube, and the tail end of the side tube is provided with a back flushing nitrogen valve;

and a second feed liquid valve is arranged on the front section of the side pipe or on the pipeline of the sampling pipe between the sample chamber and the side pipe.

In some embodiments of the present invention, the sample chamber further comprises a microporous baffle gasket, the microporous baffle gasket is located in the upper middle portion of the sample chamber, and the sample chamber is divided into an upper cavity and a lower cavity.

In some embodiments of the present invention, the microporous baffle gasket comprises, from inside to outside, a sealing inner ring, a microporous middle ring, and a sealing outer ring, wherein the microporous middle ring has a plurality of microporous ventilation rings.

In some embodiments of the present invention, the width of the ring in the micropore is 10 to 40mm, preferably 20 to 30mm, and the diameter of the micropore aeration ring is 60 to 100 mesh, preferably 60 to 80 mesh.

In some embodiments of the present invention, the upper cavity is enclosed by the upper head and the microporous baffle gasket, and the lower cavity is enclosed by the head, the cylinder and the microporous baffle gasket.

In some embodiments of the present invention, the specification of the upper head and the lower head is DN150 head/316L; the height of the cylinder body is 90-120 cm, and the diameter of the cylinder body is 150-180 cm; preferably 100 to 110cm in height and 155 to 159cm in diameter.

The utility model discloses an in some embodiments, still include the sight glass, the sight glass setting is in the intraductal upper portion of sampling tube, and what need take a sample is when the bulk drug reaction liquid, and preferred clean type does not have the residual sight glass.

In some embodiments of the present invention, the sampling tube further comprises a reinforcing plate connected between the outer wall of the sampling tube and the tube opening connecting flange.

In some embodiments of the present invention, the vacuum valve, the purge valve, the micro-pressure nitrogen valve, the back-flushing nitrogen valve, the first liquid valve, and the second liquid valve are chuck-type clean ball valves, and the specification models of the vacuum valve, the purge valve, the micro-pressure nitrogen valve, and the back-flushing nitrogen valve are DN10/PN6/316L; the specification models of the first liquid feed valve and the second liquid feed valve are DN25/PN6/316L.

In some embodiments of the present invention, the pipe orifice connecting flange is a plate type flat welding flange, and the specification is DN25/PN16//316L, and the specification of the sampling pipe is phi 32 x 4/316L.

Has the advantages that:

this sampler adopts airtight sample, has stopped the uncovered cross contamination risk that brings of outside from the source, and convenient operation is simple, and work efficiency is high. The microporous baffle plate gasket is an improvement item of the vacuum liquid sampler, and has simple structure and convenient installation; the gas in the sample chamber and the auxiliary pipeline is taken away by vacuum through the micropore ring, a vacuum atmosphere is created, and the sampling process is completed through the switches of the first valve and the second valve. After sampling is finished, the sample chamber of the sampler can be selectively disassembled and cleaned according to the process requirements, and cross contamination is avoided.

Drawings

Fig. 1 shows a schematic structural diagram of a vacuum liquid sampler according to an embodiment of the present invention, wherein the corresponding relationship between the reference numbers and the components is: 1 sample chamber, 101 lower chamber, 102 upper chamber, 103 micropore baffle, 04 upper cover, 105 lower cover, 106 barrels, 103 micropore baffle gasket, 2 sampling tubes, 201 mouth of pipe flange, 202 first feed liquid valve, 203 sight glass, 204 reinforcing plate, 3 vacuum tubes, 301 vacuum valve, 4 scavenge pipes, 401 scavenge valve, 5 minute-pressure nitrogen gas pipe, 501 minute-pressure nitrogen gas valve, 6 side pipes, 601 sampling bottle, 602 blowback nitrogen gas valve, 603 second feed liquid valve.

Fig. 2 shows a schematic structural view of a microporous baffle gasket according to an embodiment of the present invention, wherein the corresponding relationship between the reference numbers and the components is: 1031 seals the inner ring, 1032 the middle ring in the micro-hole, 1033 seals the outer ring.

Fig. 3 shows a schematic diagram of a vacuum liquid sampler and reaction vessel connection according to an embodiment of the present invention.

Fig. 4 shows a schematic structural diagram of a vacuum liquid sampler according to an embodiment of the present invention.

Detailed Description

So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those described herein. The scope of the invention is not limited, therefore, to the specific embodiments disclosed below.

In the following description, any concept relating to the directionality or orientation of up, down, left, right, inner, middle, and outer is based on the position shown in the drawings, and thus should not be construed as particularly limiting the technical solution provided by the present invention.

If do not have the particular description, the utility model discloses a quick dismantlement and the washing after the sample of being convenient for are connected to each spare part of sampler adopts flange, chuck fast-assembling, wholly can dismantle. Except that the reinforcing plate and the outer side of the mouth of pipe flange sampling tube are used for fixing the sampling tube, other parts are communicated with the sampling tube. The parts other than those forming the sample chamber are collectively referred to as accessory connectors. The pipe space formed by the auxiliary connections is called an auxiliary line.

Example 1

As shown in fig. 1, the vacuum liquid sampler includes a sample chamber 1, a sampling tube 2, a vacuum tube 3, a cleaning tube 4, a micro-pressure nitrogen gas tube 5, and a side tube 6.

The sample chamber 1 comprises, from top to bottom, an upper chamber body 102, a micro-porous baffle plate spacer 103 and a lower chamber body 101. The upper cavity 102 is enclosed by an upper seal head 104 and a micropore baffle gasket 103, and the lower cavity 101 is enclosed by a lower seal head 105, a cylinder 106 and a micropore baffle gasket 103.

The microporous baffle gasket 103 includes, from inside to outside, an inner seal ring 1031, a microporous middle ring 1032, and an outer seal ring 1033 (shown in FIG. 2). The upper cavity 102, the micropore baffle gasket 103 and the lower cavity 101 are connected by a chuck, the micropore baffle gasket 103 is formed by processing a tetrafluoro plate, and the micropore middle ring 1032 is 20mm wide and is provided with a plurality of 80-mesh micropore ventilation rings. The seal outer ring 1033 is used for the chuck to plate the gasket of the microporous baffle.

The lower parts of the vacuum tube 3, the cleaning tube 4 and the micro-pressure nitrogen tube 5 are communicated with each other and connected above the sample chamber 1, and the upper parts are respectively connected with a vacuum valve 301, a cleaning valve 401 and a micro-pressure nitrogen valve 501.

The sampling tube 2 is connected below the sample chamber 1, a sight glass 203 is arranged at the upper part in the tube of the sampling tube 2, a first feed liquid valve 202 is arranged at the middle part in the tube, and a tube opening connecting flange 201 is arranged at the lower part outside the tube of the sampling tube 2. A reinforcing plate 204 is arranged between the outer wall of the sampling tube 2 and the tube opening connecting flange 201 and is used for stabilizing the sampling tube 2.

The side pipe 6 is connected between the sample chamber 1 and the sampling pipe 2, and the side pipe 6 is sequentially provided with a second feed liquid valve 603, a sampling bottle 601 and a back flushing nitrogen valve 602 from left to right.

The specification and model of part of components are as follows:

the connection mode of the vacuum liquid closed sampler and the reaction kettle is shown in figure 3. The using method comprises the following steps:

1) Inserting a sampling tube 2 of the sampler below the liquid level of liquid in the reaction kettle through a reaction kettle opening, and keeping a certain distance between the inserted part of the sampling tube 2 and a stirring paddle of the reaction kettle to ensure that the sampling tube and the stirring paddle do not collide;

2) Connecting the pipe orifice connecting flange 201 with a flange of the reaction kettle, fastening bolts and ensuring that the sampler does not shake;

3) The pipe orifices of the vacuum pipe 3, the cleaning pipe 4 and the micro-pressure nitrogen pipe 5 of the sampler and the nitrogen back-blowing pipe 602 are respectively connected with a vacuum source, a cleaning liquid source, a micro-pressure nitrogen source and a high-pressure nitrogen source in a public system in sequence to ensure that the sealing is free from leakage;

4) Firstly, a sampling bottle 601 is installed, then a first material liquid valve 202 is closed, then a vacuum valve 301 is opened to enable a cavity 1 and an accessory connecting piece of the sampler to be vacuumized, then the vacuum valve 301 is closed, then the first material liquid valve 202 is opened, liquid in the reaction kettle is sucked into the cavity 1 under the action of vacuum, after the pressure of the system is balanced, the first material liquid valve 202 is closed, then a micro-pressure nitrogen valve 501 is opened to supplement nitrogen for the system, then a second material liquid valve 603 is opened to slowly fill the material into the sampling bottle 601, after sampling is finished, the first material liquid valve 202 is opened again to return redundant materials into the reaction kettle, finally a high-pressure nitrogen valve 602 is opened, residual liquid in the sampler is reversely blown back into the reaction kettle through nitrogen, and the system is ensured to have no residue.

5) The sampler is washd, according to production washing requirement, opens 401 after the sample, washs the valve to the sampling system on-line, and the liquid after the washing is collected through the bottom valve and is handled.

When the vacuum pumping is carried out, the gas in the sampler is taken away by the vacuum through the micropore ring to form a vacuum atmosphere.

During sampling, the sampling vacuum cavity is large in size, after pressure balance is formed, the liquid level in the vacuum cavity is about 1/2 of the vacuum cavity or lower, all liquid is located in the lower cavity, and the microporous baffle plate gasket can prevent liquid possibly generated in vacuumizing from splashing, so that a pipe orifice at the top end of the sample cavity is polluted, and sample cross contamination caused by liquid material residue is avoided. The volume of the vacuum chamber and the attached tubing is fixed so that the amount of liquid drawn by each vacuum is fixed.

Whether material enters the lower cavity 101 can be seen through the material sight glass 203.

Example 2:

as shown in fig. 4, the vacuum liquid sampler of example 2 is similar to that of example 1 except that a second feed valve 603 is provided in the conduit of sampling tube 2 between sample chamber 1 and side tube 6.

When the sampling device is used, the first material liquid valve 202 is closed, the back flushing nitrogen valve 602 is closed, the sampling bottle is installed on the sampling bottle connecting port 601, the second material liquid valve 603 is opened, the vacuum valve 301 is opened, and vacuum pumping is carried out; after vacuum is formed in the sampler, the vacuum valve 301 is closed, the first liquid material valve 202 is opened, and liquid in the reaction kettle is quantitatively sucked into the lower cavity 101; closing the second liquid material valve 603, opening the back-blowing nitrogen gas valve 602, and blowing the liquid below the second liquid material valve 603 back to the reaction kettle; closing the first liquid material valve 202, slowly opening the second liquid material valve 603, closing the sampling bottle 601 after the liquid material in the lower cavity 101 flows into the sampling bottle, taking down the sampling bottle, and opening the first liquid material valve 202 to blow back the nitrogen gas valve 602 to blow back the residual liquid material to the reaction kettle.

Example 3:

example 3 is similar to the vacuum liquid sampler of example 1 except that reinforcing plate 204 is not present.

Example 4

Example 4 is similar to the vacuum liquid sampler of example 1 except that the lower parts of the vacuum tube 3, the cleaning tube 4, and the micro-pressure nitrogen gas tube 5 are directly connected to the upper part of the sample chamber 1.

All documents mentioned in this application are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the above teachings of the present invention, and such equivalents also fall within the scope of the appended claims.

Claims

1. A vacuum liquid sampler comprises a sample chamber, a sampling tube, a vacuum tube, a cleaning tube, a micro-pressure nitrogen tube and a side tube,

the sampling tube is connected below the sample chamber, a first feed liquid valve is arranged in the middle of the sampling tube, and a tube opening connecting flange is arranged at the lower part of the sampling tube;

the side tube is connected between the sample chamber and the sampling tube, a sampling bottle is arranged below the middle section of the side tube, and the tail end of the side tube is provided with a back flushing nitrogen valve;

and a second liquid feed valve is arranged on the front section of the side pipe or the pipeline of the sampling pipe between the sample chamber and the side pipe.

2. The sampler of claim 1, further comprising a microporous baffle gasket in the sample chamber, wherein the microporous baffle gasket is located in the middle upper part of the sample chamber and divides the sample chamber into an upper cavity and a lower cavity.

3. The sampler of claim 2, wherein the microporous baffle gasket comprises, from inside to outside, an inner sealing ring, a microporous middle ring, and an outer sealing ring, wherein the microporous middle ring has a plurality of microporous vent rings.

4. The sampler of claim 3, wherein the width of the middle ring of the micro-hole is 10-40 mm, and the diameter of the micro-hole ventilation ring is 60-100 mesh.

5. The sampler of claim 3, wherein the width of the middle ring of the micro-hole is 20-30 mm, and the diameter of the micro-hole ventilation ring is 60-80 mesh.

6. The sampler of claim 2, wherein the upper cavity is defined by an upper head and a microporous baffle gasket, and the lower cavity is defined by a lower head, a barrel and a microporous baffle gasket.

7. The sampler of claim 6, wherein the upper and lower heads are DN150 head/316L; the height of the cylinder body is 90-120 cm, and the diameter of the cylinder body is 150-180 cm.

8. A sampler according to claim 6, in which the barrel is 100 to 110cm in height and 155 to 159cm in diameter.

9. A sampler according to claim 1, further comprising a sight glass disposed in the upper interior of the tube of the sampling tube.

10. A sampler according to claim 1, further comprising a reinforcing plate connected between the outer wall of the sampling tube and the nozzle connecting flange.

11. The sampler according to claim 1, wherein the vacuum valve, the purge valve, the micro-pressure nitrogen valve, the back-flushing nitrogen valve, the first liquid material valve and the second liquid material valve are chuck-type clean ball valves, and the specification models of the vacuum valve, the purge valve, the micro-pressure nitrogen valve and the back-flushing nitrogen valve are DN10/PN6/316L; the specification models of the first liquid feed valve and the second liquid feed valve are DN25/PN6/316L.

12. The sampler of claim 1, wherein the nozzle connecting flange is a plate type flat welding flange with specification model number DN25/PN16//316L; the specification and model of the sampling tube are