CN111458186A - Active powder sampling device, sampling method and application thereof - Google Patents

Abstract

The invention relates to the field of chemical equipment, and discloses an active powder sampling device, a sampling method and applications thereof. The device comprises a powder storage unit (1), a powder sampling unit (2) and a sample collection unit (3) connected in sequence through pipelines, and a gas filter unit (4) connected to the upper section of the powder sampling unit (2), so the A first brake valve (11) is provided on the connection line between the powder storage unit (1) and the powder sampling unit (2), and the connection line between the powder sampling unit (2) and the sample collection unit (3) There is a third brake valve (13) on it, and a replacement gas inlet pipeline is connected to the pipeline between the powder sampling unit (2) and the third brake valve (13). A fourth brake valve (14) is provided on the inlet line. The device of the invention can realize quantitative automatic sampling of active powder, the sampling process is safe and reliable, the waste caused by sampling is reduced, and the device is simple in design and simple in operation in the sampling process.

Description

Active powder sampling device, sampling method and application

technical field

The invention relates to the field of chemical equipment, in particular to an active powder sampling device, a sampling method and applications thereof.

Background technique

In the horizontal gas phase polypropylene process, a powder sampling system is set up in the first reactor and the second reactor respectively. The air lock can only take the powder samples produced in the first reactor, and the powder in the bag filter is the final product. Therefore, no matter what brand is produced, it must be sampled from the bag filter for analysis. When the device is in normal operation, it needs to take powder and analyze it every two hours; when the device starts, switches brands or fluctuates, it needs to sample and analyze every hour. Therefore, the powder sampling device is an important part of daily operation, and it is also a control device. The key link of product quality.

The amount of sample required for this process analysis is small, but in order to avoid clogging of the sampling line, the sampling line generally adopts a relatively thick pipe diameter, which leads to a lot of waste of powder. In addition, the powder contains triethylaluminum and non-deactivated catalyst. When it comes into direct contact with the air, it is easy to cause a fire accident. If it is stored in a closed space for a long time, a polymerization reaction is likely to occur, resulting in blockage of pipelines and equipment. In the sampling process, the nitrogen replacement is not standardized or the replacement is not complete, which will also cause the device to catch fire during the sampling process.

Therefore, there is a need to provide a method that enables accurate sampling and is safe to operate.

SUMMARY OF THE INVENTION

The purpose of the present invention is to overcome the problems such as safety accidents caused by personnel operation, waste of powder caused by each sampling, and the like, and provides a sampling device for active powder, a sampling method and application thereof. It can accurately set the sampling amount, sampling time and nitrogen replacement time, realize quantitative automatic sampling of active powder, effectively reduce the waste caused by powder sampling, and avoid fire and explosion accidents caused by incomplete nitrogen replacement of sampling, and the device is simple in design. , the sampling process is simple to operate.

In order to achieve the above object, one aspect of the present invention provides an active powder sampling device, wherein the device includes a powder storage unit, a powder sampling unit and a sample collection unit connected in sequence through pipelines, and a powder sampling unit connected to the upper section. gas filter unit,

A first brake valve is provided on the connection line between the powder storage unit and the powder sampling unit, and a third brake valve is provided on the connection line between the powder sampling unit and the sample collection unit. A replacement gas inlet pipeline is connected to the pipeline between the unit and the third brake valve, and a fourth brake valve is provided on the replacement gas inlet pipeline.

Preferably, a second brake valve is provided on the connecting line between the powder storage unit and the powder sampling unit.

Preferably, the device further comprises: a control unit for controlling the first brake valve, the third brake valve and the fourth brake valve.

Preferably, the control unit is used to control the second brake valve.

Preferably, the inner diameter of the connecting line between the powder storage unit and the powder sampling unit is 15-70 cm.

Preferably, the distance between the first brake valve and the second brake valve is 10-50 cm.

The second aspect of the present invention provides a method for sampling active powder samples, wherein the method adopts the active powder sampling device of the present invention.

Preferably, the gas introduced into the replacement gas pipeline is nitrogen, argon or carbon dioxide.

The second aspect of the present invention provides the application of the method of the present invention in sampling active powder samples.

Preferably, the active powder is polypropylene powder.

Preferably, the polypropylene powder is gas-phase reaction polypropylene powder.

Through the above technical scheme, quantitative automatic sampling of active powder can be realized, waste caused by sampling of active powder can be effectively reduced, fire and explosion accidents caused by incomplete nitrogen replacement of sampling can be avoided, and the device is simple in design and easy to operate during sampling.

Description of drawings

1 is a schematic structural diagram of an active powder sampling device provided by an embodiment of the present invention;

FIG. 2 is a schematic structural diagram of an active powder sampling device provided by another embodiment of the present invention.

Description of reference numerals

1. Powder storage unit 2. Powder sampling unit

3. Sample collection unit 4. Gas filter unit

11. The first brake valve 12. The second brake valve

13. The third brake valve 14. The fourth brake valve

Detailed ways

The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, but not to limit the present invention.

The endpoints of ranges and any values disclosed herein are not limited to the precise ranges or values, which are to be understood to encompass values proximate to those ranges or values. For ranges of values, the endpoints of each range, the endpoints of each range and the individual point values, and the individual point values can be combined with each other to yield one or more new ranges of values that Ranges should be considered as specifically disclosed herein.

In the present invention, unless otherwise stated, the use of orientation words such as "up, down, left and right" generally refers to the upper, lower, left and right in the drawings, and "inside, outside" means Corresponds to the inside and outside of the structure.

In the first aspect, the present invention provides an active powder sampling device, which comprises a powder storage unit 1, a powder sampling unit 2 and a sample collection unit 3 connected in sequence through pipelines, and a powder sampling unit 2 connected to the upper section. Gas filter unit 4, a first brake valve 11 is provided on the connection line between the powder storage unit 1 and the powder sampling unit 2, and a first brake valve 11 is provided on the connection line between the powder sampling unit 2 and the sample collection unit 3. Three brake valves 13, a replacement gas inlet pipeline is connected to the pipeline between the powder sampling unit 2 and the third brake valve 13, and a fourth brake valve is arranged on the replacement gas inlet pipeline 14. FIG. 1 is a schematic structural diagram of an active powder sampling device according to an embodiment of the present invention. As shown in Figure 1, the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, the gas filter unit 4 is connected to the upper section of the powder sampling unit 2, and the powder storage unit 1 is connected to the powder sampling unit 2. A first brake valve 11 is arranged on the connecting pipeline, a third brake valve 13 is arranged on the connecting pipeline between the powder sampling unit 2 and the sample collection unit 3, and the connection between the powder sampling unit 2 and the third brake valve 13 is provided. A replacement gas inlet pipeline is connected to the pipeline, and a fourth brake valve 14 is arranged on the replacement gas inlet pipeline.

The active powder sampling device of the present invention can control the sampling process, sampling amount, sampling time and replacement gas operation by arranging brake valves on the connecting pipelines of each unit, thereby reducing the waste of powder materials caused by each sampling , reducing the workload of on-site operators, improving the economic benefits of the entire process, and avoiding fire and explosion accidents caused by incomplete nitrogen replacement for sampling, and the equipment is simple in design, low in one-time investment in equipment, and simple in sampling process operation. Realize automatic quantitative collection of active powder samples.

In order to further ensure accurate sampling and reduce waste in the sampling process, in the present invention, preferably, a second brake valve 12 is provided on the connecting line between the powder storage unit 1 and the powder sampling unit 2 . By adding a second brake valve 12 on the connecting line between the powder storage unit 1 and the powder sampling unit 2, the controllability of the sampling amount is further realized. As shown in Figure 2, the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, the gas filter unit 4 is connected to the upper section of the powder sampling unit 2, and the powder storage unit 1 is connected to the powder sampling unit 2. A first brake valve 11 and a second brake valve 12 are arranged on the connecting pipeline in sequence, a third brake valve 13 is arranged on the connecting pipeline between the powder sampling unit 2 and the sample collection unit 3, and the powder sampling unit 2 is connected to the third brake valve 13. The pipeline between the three brake valves 13 is connected with a replacement gas inlet pipeline, and a fourth brake valve 14 is arranged on the replacement gas inlet pipeline.

In order to further realize the controllability of sampling amount, sampling time, sampling time and replacement gas operation in the sampling process, in the present invention, preferably, the device further includes: a control unit for controlling the first brake valve 11 , the third brake valve 13 and the fourth brake valve 14 . The control unit realizes the control of the first brake valve 11, the third brake valve 13 and the fourth brake valve 14, so as to further ensure that the sample amount obtained can meet the requirements of normal product analysis, and at the same time, the sampling replacement process is controlled by Set the sequence control of Cheng Xun to ensure the effect of replacement.

Preferably, the control unit is used to control the second brake valve 12 . The control of the second brake valve 12 is realized by the control unit, which can further ensure the amount of powder flowing between the first brake valve 11 and the second brake valve 12, and realize the precise control of the sampling amount.

In order to further avoid the waste of powder material during the sampling process, in the invention, preferably, the inner diameter of the connecting pipeline between the powder material storage unit 1 and the powder material sampling unit 2 is 15-70 cm; more preferably, the powder material The inner diameter of the connecting line between the storage unit 1 and the powder sampling unit 2 is 20-65 cm. Compared with the thicker pipeline used in the existing device to avoid the blockage of the sampling pipeline, which leads to a lot of waste of powder, by using the connecting pipeline with a smaller inner diameter, the amount of sample required for analysis is met, and the powder is further reduced. waste.

In order to further ensure the sampling amount, in the present invention, preferably, the distance between the first brake valve 11 and the second brake valve 12 is 10-50 cm; more preferably, the first brake valve 11 The distance from the second brake valve 12 is 20-40 cm. By controlling the distance between the first brake valve 11 and the second brake valve 12, the amount of samples taken in the pipeline is further ensured.

In a second aspect, the present invention provides a method for sampling an active powder sample, which adopts the above-mentioned active powder sampling device.

In the specific implementation of the present invention, the active powder sampling device shown in FIG. 1 is used, the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, and the gas filter unit 4 is connected to the powder sampling unit 2 In the upper section, a first brake valve 11 is provided on the connecting line between the powder storage unit 1 and the powder sampling unit 2, and a third brake valve 13 is provided on the connecting line between the powder sampling unit 2 and the sample collection unit 3. A replacement gas inlet pipeline is connected to the pipeline between the material sampling unit 2 and the third brake valve 13 , and a fourth brake valve 14 is arranged on the replacement gas inlet pipeline. The on/off and start-up time of each brake valve are automatically or manually controlled by the control unit. Specifically, in the initial state, the first brake valve 11, the fourth brake valve 14 and the third brake valve 13 are in a closed state, Open the first brake valve 11, the powder enters the powder sampling unit 2 after passing through the first brake valve 11, close the first brake valve 11 and open the fourth brake valve 14, and pass nitrogen to replace the gas phase in the sample After closing the fourth brake valve 14, the gas carried by the powder is discharged to the torch through the gas filter unit 4. After the sample is collected, the third brake valve 13 is opened to release the sample into the sample collection unit 3, and the sampling is completed. By controlling the opening/closing time of the first brake valve 11, the sampling amount of the sample can be controlled, and the controllable and automatic sampling of the sampling time can be realized.

In the specific implementation of the present invention, the active powder sampling device shown in FIG. 2 is used, the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, and the gas filter unit 4 is connected to the powder sampling unit 2 In the upper section, the connecting line between the powder storage unit 1 and the powder sampling unit 2 is provided with a first brake valve 11 and a second brake valve 12, and the connecting line between the powder sampling unit 2 and the sample collection unit 3 is provided with a first brake valve 11 and a second brake valve 12. Three brake valves 13, the pipeline between the powder sampling unit 2 and the third brake valve 13 is connected with a replacement gas inlet pipeline, and a fourth brake valve 14 is arranged on the replacement gas inlet pipeline. The on/off, start-up time and on/off interval of each brake valve are automatically or manually controlled by the control unit. Specifically, in the initial state, the first brake valve 11 , the fourth brake valve 14 and the third brake valve The brake valve 13 is closed and the second brake valve 12 is open. Open the first brake valve 11 and close the second brake valve 12. After the powder passes through the first brake valve 11, the first brake valve 11 is closed and the second brake valve 12 is closed. Open the second brake valve 12, so that the powder enters the powder sampling unit 2 through the second brake valve 12, then close the second brake valve 12 and open the fourth brake valve 14 to pass nitrogen to replace the gas phase in the sample After closing the fourth brake valve 14, the gas carried by the powder is discharged to the torch through the gas filter unit 4. After the sample is collected, the third brake valve 13 is opened to release the sample into the sample collection unit 3, and the sampling is completed. By controlling the on/off time of the first brake valve 11 and the second brake valve 12, the sampling amount is further controllable, and the waste of powder material caused by sampling is reduced; The pipeline distance between the second brake valves 12 further realizes the controllability of the sampling amount.

In the method of the present invention, preferably, the gas introduced into the replacement gas pipeline is nitrogen, argon or carbon dioxide. In a specific embodiment of the present invention, nitrogen gas is used for displacement.

The above nitrogen replacement time is not particularly limited, and those skilled in the art can select according to actual needs. In the specific embodiment of the present invention, the nitrogen replacement time is 30-60 seconds, but not limited thereto.

In the third invention, the present invention provides the application of the above method in sampling active powder samples.

In the application of the invention, the active powder is polypropylene powder.

In the application of the invention, the polypropylene powder is gas-phase reaction polypropylene powder.

The present invention will be described in detail below by means of examples. In the following examples, unless otherwise specified, all materials used can be obtained commercially, and unless otherwise specified, the used methods are conventional methods in the field.

Example 1

The active powder sampling device shown in Figure 2 is used, wherein the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, the gas filter unit 4 is connected to the upper section of the powder sampling unit 2, and the powder storage A first brake valve 11 and a second brake valve 12 are arranged on the connecting line between the unit 1 and the powder sampling unit 2, and a third brake valve 13 is arranged on the connecting line between the powder sampling unit 2 and the sample collection unit 3 , the pipeline between the powder sampling unit 2 and the third brake valve 13 is connected with a replacement gas inlet pipeline, and the replacement gas inlet pipeline is provided with a fourth brake valve 14, wherein the powder storage unit 1 and the powder The inner diameter of the connecting pipeline of the material sampling unit 2 is 50 cm, and the distance between the first braking valve 11 and the second braking valve 12 is 30 cm.

The sampling method of active powder samples is as follows:

Step 1: Standby state. At this time, the first brake valve 11 , the fourth brake valve 14 and the third brake valve 13 are closed, and the second brake valve 12 is opened.

Step 2: Powder collection. First, close the second brake valve 12. When the control unit receives the closing signal of the second brake valve 12, the first brake valve 11 is opened for a predetermined time (the opening/closing interval is 1 second) and then closed; When the closing signal of the first brake valve 11 is reached, the second brake valve 12 is opened.

Step 3: Nitrogen replacement. The fourth brake valve 14 is opened, and after nitrogen gas replaces the gas phase in the sample for 50 seconds, the fourth brake valve 14 is closed, and the gas carried by the powder is discharged to the torch through the gas filter unit 4 .

Step 4: Sampling is complete. At this time, the first brake valve 11 and the fourth brake valve 14 are closed, the second brake valve 12 is opened, and the sample is stored in the powder sampling unit 2 , and the field operator takes the sample by opening the third brake valve 13 .

Wherein, the opening/closing and opening/closing interval time of each brake valve are automatically or manually controlled by the control unit. It is also possible to switch to manual control to open/close the first brake valve 11 and the second brake valve 12, and then open the fourth brake valve according to the situation on site (when the sampling line is blocked or a large amount of powder samples are required). 14 Use nitrogen to unclog the sampling line or displace the gas in bulk powder samples.

Example 2

Using the active powder sampling device shown in FIG. 1, the powder storage unit 1 is connected to the powder sampling unit 2 and the sample collection unit 3 in sequence, the gas filter unit 4 is connected to the upper section of the powder sampling unit 2, and the powder storage unit 1 is connected to A first brake valve 11 is provided on the connecting line of the powder sampling unit 2, a third brake valve 13 is provided on the connecting line between the powder sampling unit 2 and the sample collection unit 3, and the powder sampling unit 2 is connected to the third system. The pipeline between the dynamic valves 13 is connected with a replacement gas inlet pipeline, and a fourth brake valve 14 is arranged on the replacement gas inlet pipeline, wherein the inner diameter of the connecting pipeline between the powder storage unit 1 and the powder sampling unit 2 is 50cm.

The sampling method of active powder samples is as follows:

Step 1: Standby state. At this time, the first brake valve 11 , the fourth brake valve 14 and the third brake valve 13 are closed.

Step 2: Powder collection. First, the first brake valve 11 is opened for a predetermined time (the opening/closing interval is 1 second) and then closed.

Step 3: Nitrogen replacement. The fourth brake valve 14 is opened, and after nitrogen gas replaces the gas phase in the sample for 50 seconds, the fourth brake valve 14 is closed, and the gas carried by the powder is discharged to the torch through the gas filter unit 4 .

Step 4: Sampling is complete. At this time, the first brake valve 11 and the fourth brake valve 14 are closed, the samples are stored in the powder sampling unit 2 , and the samples are taken out by opening the third brake valve 13 .

Wherein, the opening/closing and opening/closing interval time of each brake valve are automatically or manually controlled by the control unit. It is also possible to open/close the first brake valve 11 by switching to manual control, and then open the fourth brake valve 14 to dredge the sampling line with nitrogen gas or Displace gas in bulk powder samples.

Compared with the currently applied sampling system, after the quantitative automatic sampling system is adopted, the amount of waste remaining after each sampling is significantly reduced, the operating cost of the device is reduced, and the economic benefit of the entire device is improved; The frequency will also be greatly reduced, effectively reducing the workload of on-site operators and saving labor costs; the nitrogen replacement time is set through the program to avoid safety accidents caused by personnel operations.

The preferred embodiments of the present invention have been described above in detail with reference to the accompanying drawings, however, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, including the combination of various specific technical features in any suitable manner. In order to avoid unnecessary repetition, the present invention will not describe various possible combinations. However, these simple modifications and combinations should also be regarded as the contents disclosed in the present invention, and all belong to the protection scope of the present invention.

Claims (10)

1. An active powder sampling device is characterized by comprising a powder storage unit (1), a powder sampling unit (2), a sample collecting unit (3) and a gas filtering unit (4) which are sequentially connected through pipelines, wherein the gas filtering unit (4) is connected with the upper section of the powder sampling unit (2),

the powder sampling device is characterized in that a first brake valve (11) is arranged on a connecting pipeline between the powder storage unit (1) and the powder sampling unit (2), a third brake valve (13) is arranged on a connecting pipeline between the powder sampling unit (2) and the sample collection unit (3), a replacement gas inlet pipeline is connected to a pipeline between the powder sampling unit (2) and the third brake valve (13), and a fourth brake valve (14) is arranged on the replacement gas inlet pipeline.

2. Active powder sampling device according to claim 1, wherein a second brake valve (12) is provided on the connection line of the powder storage unit (1) and the powder sampling unit (2).

3. The active powder sampling device of claim 1 or 2, wherein the device further comprises:

a control unit for controlling the first brake valve (11), the third brake valve (13) and the fourth brake valve (14);

preferably, the control unit is used for controlling the second brake valve (12).

4. Active powder sampling device according to claim 1 or 2, wherein the internal diameter of the connecting line of the powder storage unit (1) and the powder sampling unit (2) is 15-70 cm.

5. Active powder sampling device according to claim 2, wherein the distance between the first stop valve (11) and the second stop valve (12) is 10-50 cm.

6. A method for sampling an active powder sample, characterized in that the method employs the active powder sampling device according to claims 1-5.

7. The method for sampling an active powder sample according to claim 6, wherein the gas introduced into the substitution gas introduction line is nitrogen, argon or carbon dioxide.

8. Use of the method of claim 7 for sampling an active powder sample.

9. Use according to claim 8, wherein the active powder is polypropylene powder.

10. Use according to claim 9, wherein the polypropylene powder is a gas-phase reactive polypropylene powder.

Images