CN111458186A - Active powder sampling device, sampling method and application thereof - Google Patents
Active powder sampling device, sampling method and application thereof Download PDFInfo
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- CN111458186A CN111458186A CN202010275596.1A CN202010275596A CN111458186A CN 111458186 A CN111458186 A CN 111458186A CN 202010275596 A CN202010275596 A CN 202010275596A CN 111458186 A CN111458186 A CN 111458186A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1006—Dispersed solids
Abstract
The invention relates to the field of chemical equipment, and discloses an active powder sampling device, a sampling method and application thereof. The device comprises a powder storage unit (1), a powder sampling unit (2), a sample collecting unit (3) and a gas filtering unit (4) connected to the upper section of the powder sampling unit (2), wherein the powder storage unit (1) and the sample collecting unit (2) are sequentially connected through pipelines, a first brake valve (11) is arranged on a connecting pipeline of the powder storage unit (1) and the powder sampling unit (2), a third brake valve (13) is arranged on a connecting pipeline of the powder sampling unit (2) and the sample collecting unit (3), replacement gas is connected to a pipeline between the powder sampling unit (2) and the third brake valve (13) and enters the pipeline, and a fourth brake valve (14) is arranged on the replacement gas entering pipeline. The device can realize the quantitative automatic sampling of the active powder, has safe and reliable sampling process, reduces the waste caused by sampling, and has simple design and simple operation of the sampling process.
Description
Technical Field
The invention relates to the field of chemical equipment, in particular to an active powder sampling device, a sampling method and application thereof.
Background
The horizontal gas-phase polypropylene process has powder sampling systems in the first reactor and the second reactor separately, and the airlock can only take the powder sample produced in the first reactor, and the powder in the bag filter is the final powder product. When the device normally operates, powder needs to be taken out every two hours for analysis; when the device starts, the grade is switched or fluctuation occurs, sampling and analysis are needed once per hour, so that the powder sampling device is an important part of daily operation and is also a key link for controlling the product quality.
The amount of samples required by the analysis in the process is less, but in order to avoid the blockage of the sampling pipeline, the sampling pipeline generally adopts a thicker pipe diameter, so that more powder waste is caused. In addition, the powder contains triethyl aluminum and an inactivated catalyst, when the powder is directly contacted with air, fire accidents are easily caused, polymerization reaction is easily caused after the powder is stored in a closed space for a long time, pipelines and equipment are blocked, and meanwhile, because nitrogen replacement is not standard or thorough in the manual sampling process of personnel, the ignition accidents of the device in the sampling process can also be caused.
Therefore, it is desirable to provide a method that enables accurate sampling and safe operation.
Disclosure of Invention
The invention aims to solve the problems of safety accidents caused by personnel operation, powder waste caused by each sampling and the like in the prior art, and provides an active powder sampling device, a sampling method and application thereof.
In order to achieve the above object, the present invention provides an active powder sampling apparatus, wherein the apparatus comprises a powder storage unit, a powder sampling unit and a sample collection unit connected in sequence by a pipeline, and a gas filtration unit connected to the upper section of the powder sampling unit,
the powder sampling device is characterized in that a first brake valve is arranged on a connecting pipeline between the powder storage unit and the powder sampling unit, a third brake valve is arranged on a connecting pipeline between the powder sampling unit and the sample collecting unit, a replacement gas inlet pipeline is connected to a pipeline between the powder sampling unit and the third brake valve, and a fourth brake valve is arranged on the replacement gas inlet pipeline.
Preferably, a second brake valve is arranged on a connecting pipeline of the powder storage unit and the powder sampling unit.
Preferably, the apparatus further comprises: and the control unit is used for controlling the first brake valve, the third brake valve and the fourth brake valve.
Preferably, the control unit is configured to control the second brake valve.
Preferably, the inner diameter of the connecting pipeline of 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 invention provides a sampling method of an active powder sample, wherein the method adopts the active powder sampling device.
Preferably, the gas introduced into the replacement gas introduction line is nitrogen, argon or carbon dioxide.
In a second aspect, the invention provides the use of the method of the invention for sampling an active powder sample.
Preferably, the active powder is polypropylene powder.
Preferably, the polypropylene powder is a gas-phase reaction polypropylene powder.
Through above-mentioned technical scheme, can realize the automatic sample of ration of active powder, effectively reduce the waste that active powder sampling leads to, avoid because of conflagration, the explosion accident that the replacement of sample nitrogen gas thoroughly leads to, and the device design is simple, and the sampling process is easy and simple to handle.
Drawings
FIG. 1 is a schematic structural diagram of an active powder sampling device according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an active powder sampling device according to another embodiment of the present invention.
Description of the reference numerals
1. Powder storage unit 2 and powder sampling unit
3. Sample collection unit 4, gas filtration unit
11. First brake valve 12, second brake valve
13. Third brake valve 14, fourth brake valve
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, the use of directional terms such as "upper, lower, left, right" generally means upper, lower, left, right in the drawings, and "inner, outer" means inner and outer of the corresponding structures, unless otherwise specified.
In a first aspect, the invention provides an active powder sampling device, which comprises a powder storage unit 1, a powder sampling unit 2, a sample collecting unit 3 and an air filtering unit 4 connected to the upper section of the powder sampling unit 2, which are sequentially connected through pipelines, wherein 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 collecting 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. Fig. 1 is a schematic structural diagram of an active powder sampling device according to an embodiment of the present invention. As shown in fig. 1, the powder storage unit 1 is sequentially connected with the powder sampling unit 2 and the sample collection unit 3, the gas filtration unit 4 is connected to the upper section of the powder sampling unit 2, 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.
According to the active powder sampling device, the brake valves are arranged on the connecting pipelines of all units, so that the control of the sampling process, the sampling amount, the sampling time and the gas replacement operation is realized, the powder waste caused by each sampling is reduced, the workload of field operators is reduced, the economic benefit of the whole process is improved, meanwhile, fire and explosion accidents caused by incomplete sampling nitrogen replacement are avoided, the equipment is simple in design, the one-time investment of the equipment is very low, the sampling process is simple to operate, and the automatic quantitative collection of active powder samples can be realized.
In order to further ensure accurate sampling and reduce waste generated during sampling, in the present invention, it is preferable that a second brake valve 12 is provided on a connection line between the powder storage unit 1 and the powder sampling unit 2. The control of the sampling amount is further realized by additionally arranging a second brake valve 12 on a connecting pipeline of the powder storage unit 1 and the powder sampling unit 2. As shown in fig. 2, the powder storage unit 1 is sequentially connected with the powder sampling unit 2 and the sample collection unit 3, the gas filtration unit 4 is connected to the upper section of the powder sampling unit 2, a first brake valve 11 and a second brake valve 12 are sequentially 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.
In order to further realize the controllability of the sampling amount, the sampling time and the operation of the displacement gas during the sampling process, in the present invention, preferably, the apparatus further comprises: and the control unit is used for controlling the first brake valve 11, the third brake valve 13 and the fourth brake valve 14. The control of the first brake valve 11, the third brake valve 13 and the fourth brake valve 14 is realized through the control unit, the obtained sample amount can be further ensured to meet the requirement of normal product analysis, meanwhile, the control is realized on the sampling replacement process, and the replacement effect is ensured through the sequential control of the set program.
Preferably, the control unit is configured to control the second brake valve 12. The control unit is used for controlling the second brake valve 12, so that the amount of powder flowing between the first brake valve 11 and the second brake valve 12 can be further ensured, and the sampling amount can be accurately controlled.
In order to further avoid powder waste caused in the sampling process, in the invention, preferably, the inner diameter of the connecting pipeline of the powder storage unit 1 and the powder sampling unit 2 is 15-70 cm; more preferably, the inner diameter of the connecting line of the powder storage unit 1 and the powder sampling unit 2 is 20-65 cm. Compared with the prior device which adopts a thicker pipeline to avoid the blockage of the sampling pipeline, the device has the advantages that the powder waste is more, and the powder waste is further reduced while the sample amount required by analysis is met by adopting the connecting pipeline with the thinner inner diameter.
In order to further ensure the sampling amount, in the present invention, it is preferable that the distance between the first and second stop valves 11 and 12 is 10 to 50 cm; more preferably, the distance between the first brake valve 11 and 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 sample taken in the line is further ensured.
In a second aspect, the invention provides a method for sampling an active powder sample, which adopts the active powder sampling device.
In the specific implementation of the invention, the active powder sampling device shown in fig. 1 is adopted, the powder storage unit 1 is sequentially connected with the powder sampling unit 2 and the sample collection unit 3, the gas filtering unit 4 is connected with the upper section of the powder sampling unit 2, a first brake valve 11 is arranged on a connecting pipeline of the powder storage unit 1 and the powder sampling unit 2, a third brake valve 13 is arranged on a connecting pipeline of the powder sampling unit 2 and the sample collection unit 3, a replacement gas inlet pipeline is connected on 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. The on/off and starting time of each brake valve are automatically or manually controlled through a control unit, specifically, in an initial state, the first brake valve 11, the fourth brake valve 14 and the third brake valve 13 are in a closed state, the first brake valve 11 is opened, powder enters the powder sampling unit 2 after passing through the first brake valve 11, the first brake valve 11 is closed, the fourth brake valve 14 is opened, nitrogen is introduced to replace the gas phase in a sample, the fourth brake valve 14 is closed, the gas carried by the powder is discharged to a torch through the gas filtering unit 4, after the sample is collected, the third brake valve 13 is opened to discharge the sample to the sample collecting unit 3, the sampling is completed, the sampling amount of the sample can be controlled by controlling the on/off time of the first brake valve 11, and the controllable and automatic sampling of the sampling time can be realized.
In the specific implementation of the invention, the active powder sampling device shown in fig. 2 is adopted, the powder storage unit 1 is sequentially connected with the powder sampling unit 2 and the sample collection unit 3, the gas filtering unit 4 is connected with the upper section of the powder sampling unit 2, a first brake valve 11 and a second brake valve 12 are arranged on a connecting pipeline of the powder storage unit 1 and the powder sampling unit 2, a third brake valve 13 is arranged on a connecting pipeline of the powder sampling unit 2 and the sample collection unit 3, a replacement gas inlet pipeline is connected on 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. The opening/closing, the starting time and the opening/closing interval time of each brake valve are automatically or manually controlled by a control unit, specifically, in an initial state, a first brake valve 11, a fourth brake valve 14 and a third brake valve 13 are in a closed state, a second brake valve 12 is in an open state, the first brake valve 11 is opened to close the second brake valve 12, powder passes through the first brake valve 11, the first brake valve 11 is closed and the second brake valve 12 is opened, so that the powder enters a powder sampling unit 2 through the second brake valve 12, the second brake valve 12 is closed, the fourth brake valve 14 is opened to introduce nitrogen to replace the gas phase in the sample, the fourth brake valve 14 is closed, the gas carried by the powder is discharged to a torch through a gas filtering unit 4, after the sample is collected, the third brake valve 13 is opened to discharge the sample to a sample collecting unit 3 to finish the sampling, by controlling the on/off time of the first brake valve 11 and the second brake valve 12, the sampling quantity is further controllable, and the waste of powder caused by sampling is reduced; in addition, the sampling amount can be further controlled by controlling the line distance between the first brake valve 11 and the second brake valve 12.
In the method of the present invention, preferably, the gas introduced into the replacement gas introduction line is nitrogen, argon or carbon dioxide. In a specific embodiment of the present invention, nitrogen gas is used for the substitution.
The nitrogen gas replacement time is not particularly limited, and may be selected by those skilled in the art according to actual needs, and in the embodiment of the present invention, the nitrogen gas replacement time is 30 to 60 seconds, but is not limited thereto.
In a third aspect, the present invention provides the use of the above method for sampling an active powder sample.
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 way of examples. In the following examples, each material used was commercially available unless otherwise specified, and the method used was a conventional method in the art unless otherwise specified.
Example 1
The active powder sampling device shown in fig. 2 is adopted, wherein a powder storage unit 1 is sequentially connected with a powder sampling unit 2 and a sample collecting unit 3, an air filtering unit 4 is connected with the upper section of the powder sampling unit 2, a first brake valve 11 and a second brake valve 12 are arranged on a connecting pipeline of the powder storage unit 1 and the powder sampling unit 2, a third brake valve 13 is arranged on a connecting pipeline of the powder sampling unit 2 and the sample collecting 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, wherein the inner diameter of the connecting pipeline between the powder storage unit 1 and the powder sampling unit 2 is 50cm, and the distance between the first brake valve 11 and the second brake valve 12 is 30 cm.
The sampling method of the active powder sample comprises the following steps:
step 1: and a 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: and (5) collecting powder. Firstly, closing the second brake valve 12, and when the control unit receives a closing signal of the second brake valve 12, closing the first brake valve 11 after opening for a preset time (the opening/closing interval time is 1 second); when the control unit receives a closing signal of the first brake valve 11, the second brake valve 12 is opened.
And step 3: and (4) replacing with nitrogen. After the fourth brake valve 14 was opened and the gas phase in the sample was replaced with nitrogen for 50 seconds, the fourth brake valve 14 was closed and the gas carried by the powder was discharged to a torch through the gas filtration unit 4.
And 4, step 4: and (5) finishing sampling. At this time, the first brake valve 11 and the fourth brake valve 14 are closed, the second brake valve 12 is opened, the sample is stored in the powder sampling unit 2, and the site operator takes the sample by opening the third brake valve 13.
Wherein the on/off and the on/off interval time of each brake valve are automatically or manually controlled by a control unit. It is also possible to open/close the first brake valve 11 and the second brake valve 12 by switching to manual control according to the field situation (when the sampling line is clogged or a large amount of powder sample is required), and then open the fourth brake valve 14 to dredge the sampling line with nitrogen or to replace the gas in the large amount of powder sample.
Example 2
Adopt the active powder sampling device shown in fig. 1, powder storage unit 1 connects gradually with powder sampling unit 2 and sample collection unit 3, gas filtration unit 4 connects in the upper segment of powder sampling unit 2, be equipped with first brake valve 11 on the connecting line of powder storage unit 1 and powder sampling unit 2, be equipped with third brake valve 13 on the connecting line of powder sampling unit 2 and sample collection unit 3, be connected with replacement gas on the pipeline between powder sampling unit 2 and the third brake valve 13 and let in the pipeline, be equipped with fourth brake valve 14 on the replacement gas lets in the pipeline, wherein, the internal diameter of the connecting line of powder storage unit 1 and powder sampling unit 2 is 50 cm.
The sampling method of the active powder sample comprises the following steps:
step 1: and a 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: and (5) collecting powder. The first brake valve 11 is first opened for a predetermined time (the open/close interval time is 1 second) and then closed.
And step 3: and (4) replacing with nitrogen. After the fourth brake valve 14 was opened and the gas phase in the sample was replaced with nitrogen for 50 seconds, the fourth brake valve 14 was closed and the gas carried by the powder was discharged to a torch through the gas filtration unit 4.
And 4, step 4: and (5) finishing sampling. At this time, the first brake valve 11 and the fourth brake valve 14 are closed, and the sample is stored in the powder sampling unit 2 and is taken out by opening the third brake valve 13.
Wherein the on/off and the on/off interval time of each brake valve are automatically or manually controlled by a 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 unblock the sampling line with nitrogen or to replace the gas in a large amount of powder samples according to the field situation (when the sampling line is clogged or a large amount of powder samples are required).
Compared with the sampling system applied at present, after the quantitative automatic sampling system is adopted, the amount of the waste materials left after each sampling is obviously reduced, the operating cost of the device is reduced, and the economic benefit of the whole device is improved; the frequency of cleaning the waste material tank by field operators is greatly reduced, the workload of the field operators is effectively reduced, and the labor cost is saved; the time for replacing the nitrogen is set through a program, so that safety accidents caused by personnel operation are avoided.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, numerous simple modifications can be made to the technical solution of the invention, including combinations of the individual specific technical features in any suitable way. The invention is not described in detail in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
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.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010275596.1A CN111458186A (en) | 2020-04-09 | 2020-04-09 | Active powder sampling device, sampling method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010275596.1A CN111458186A (en) | 2020-04-09 | 2020-04-09 | Active powder sampling device, sampling method and application thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3556730A (en) * | 1968-10-21 | 1971-01-19 | Phillips Petroleum Co | Sampling system |
| CN1184529A (en) * | 1995-05-11 | 1998-06-10 | 博雷利丝·波利默斯公司 | Method and apparatus for taking sample |
| CN1296018A (en) * | 1999-11-11 | 2001-05-23 | 联合碳化化学品及塑料技术公司 | Sampler for fluidized bed gas-phase polymerization reaction system |
| US6592827B1 (en) * | 2000-10-24 | 2003-07-15 | Univation Technologies Llc | Sampling system for fluidized bed gas phase polymerization reaction systems |
| CN1942484A (en) * | 2004-02-13 | 2007-04-04 | 托塔尔石油化学产品研究弗吕公司 | Method for improving a polymerization reaction by taking out and analysing a sample |
| CN205027548U (en) * | 2015-06-01 | 2016-02-10 | 中国石油天然气股份有限公司 | Online sampling device |
-
2020
- 2020-04-09 CN CN202010275596.1A patent/CN111458186A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3556730A (en) * | 1968-10-21 | 1971-01-19 | Phillips Petroleum Co | Sampling system |
| CN1184529A (en) * | 1995-05-11 | 1998-06-10 | 博雷利丝·波利默斯公司 | Method and apparatus for taking sample |
| CN1296018A (en) * | 1999-11-11 | 2001-05-23 | 联合碳化化学品及塑料技术公司 | Sampler for fluidized bed gas-phase polymerization reaction system |
| US6592827B1 (en) * | 2000-10-24 | 2003-07-15 | Univation Technologies Llc | Sampling system for fluidized bed gas phase polymerization reaction systems |
| CN1942484A (en) * | 2004-02-13 | 2007-04-04 | 托塔尔石油化学产品研究弗吕公司 | Method for improving a polymerization reaction by taking out and analysing a sample |
| CN205027548U (en) * | 2015-06-01 | 2016-02-10 | 中国石油天然气股份有限公司 | Online sampling device |
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