Closed sampling system and sampling method suitable for diethyl zinc
By introducing a vacuum system, nitrogen inlet and multiple ball valves into the closed sampling system, vacuum decomposition and nitrogen flushing in the pipeline is achieved, which solves the problems of air contact and pipeline residue during diethyl zinc sampling, and significantly improves the sample Accuracy and freshness.
Patent Information
- Application Number
- CN202411415210.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-11
- Publication Date
- 2024-12-13
AI Technical Summary
When performing sampling operations on diethyl zinc, existing sealed samplers cannot avoid contact with air or residual liquid for the last sampling in the pipeline, affecting the accuracy of the second sampling sample.
A closed sampling system including a vacuum system, a nitrogen inlet and a conical bottle is designed. Through the alternating control of multiple ball valves, vacuum removal and nitrogen flushing in the pipeline are realized to avoid contact with the air or residual pipes.
It effectively improves the accuracy of secondary sampling samples and prevents contamination and sample aging during sampling.
Smart Images
Figure CN119124739A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of closed sampling, and in particular to a closed sampling system and a sampling method suitable for diethyl zinc. Background Art
[0002] In the prior art, diethyl zinc has the dangerous characteristics of spontaneous combustion in the air and violent reaction with water. In the production process, sampling and analysis of the reaction process or finished product is inevitable. Ordinary closed samplers are inevitably in contact with air or the last sampling liquid remains in the pipeline during the sampling process, affecting the accuracy of the second sampling sample. Therefore, how to design a closed sampling system that can consider both the sampling process to avoid contamination and the freshness of the sample to prevent the residue of the last sampling sample. Summary of the invention
[0003] The problem to be solved by the present application is that when the existing common closed sampler performs a sampling operation on diethyl zinc, it is inevitable that the sample will come into contact with the air or the last sampling liquid will remain in the pipeline, thereby affecting the accuracy of the second sampling sample.
[0004] In order to solve the above technical problems, the present application provides a closed sampling system suitable for diethyl zinc, including a pipeline for connecting with a reactor or a container, a plurality of ball valves for realizing opening and closing functions are arranged at intervals on the upper part of the pipeline, a conical flask for sampling operation is threadedly connected to the upper part of the pipeline, one end of the pipeline is connected to a vacuum system, and the other end of the pipeline is connected to the reactor or the container, and a nitrogen inlet for blowing nitrogen is also arranged at one end of the upper part of the pipeline close to the vacuum system.
[0005] Since the closed sampling system of the present application is designed with a pipeline with a vacuum system, a nitrogen inlet, a conical flask and a ball valve, vacuum impurity removal and nitrogen flushing operations can be achieved inside the pipeline by alternately controlling multiple ball valves, so as to avoid contact between diethyl zinc and air or residue on the upper part of the pipeline during the sampling process, thereby solving the problem that when the common closed sampler in the prior art performs a sampling operation on diethyl zinc, it is inevitable to contact with air or the last sampling liquid remains in the pipeline, thereby affecting the accuracy of the second sampling sample. BRIEF DESCRIPTION OF THE DRAWINGS
[0006] Figure 1 Schematic diagram of the process flow of the embodiment.
[0007] Figure 2 for Figure 1 A partial enlarged schematic diagram of .
[0008] In the figure: 1. sight glass; 2. first ball valve; 3. second ball valve; 4. pressure gauge; 5. third ball valve; 6. fourth ball valve; 7. fifth ball valve; 8. conical flask. DETAILED DESCRIPTION
[0009] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application. Example
[0010] The present application relates to a closed sampling system suitable for diethyl zinc, such as Figure 1-2 As shown, the closed sampling system includes a pipeline for communicating with a reactor or a container, a plurality of ball valves for realizing opening and closing functions are arranged at intervals on the upper part of the pipeline, a conical flask 8 for sampling operation is threadedly connected to the upper part of the pipeline, a toluene solution is added to the interior of the conical flask 8 in advance and weighed, diethyl zinc can be stably stored in the toluene solution and is non-hazardous, one end of the pipeline is connected to the vacuum system, and the other end of the pipeline is connected to the reactor or the container, and a nitrogen inlet for blowing nitrogen is arranged at one end of the upper part of the pipeline close to the vacuum system, and in order to be able to determine whether there is gas inside the pipeline, a pressure gauge 4 capable of monitoring the pressure inside the pipe is also provided on the upper part of the pipeline.
[0011] There are five ball valves, which are respectively divided into a first ball valve 2, a second ball valve 3, a third ball valve 5, a fourth ball valve 6 and a fifth ball valve 7. The first ball valve 2 is arranged at the upper part of the pipeline between the sight glass 1 and the pressure gauge 4, the second ball valve 3 is arranged at the upper part of the pipeline between the first ball valve 2 and the conical flask 8, the third ball valve 5 is arranged at a position on the upper part of the pipeline close to the pressure gauge 4, the fourth ball valve 6 is arranged at a position on the upper part of the pipeline close to the vacuum system, and the fifth ball valve 7 is arranged at a position on the upper part of the pipeline close to the nitrogen inlet.
[0012] The sampling method is as follows: (1) Toluene solution is pre-added into the sampling conical flask 8 and weighed, and the conical flask 8 is connected to the pipeline through a thread; (2) Keep the first ball valve 2 and the fifth ball valve 7 closed, and open the second ball valve 3, the third ball valve 5 and the fourth ball valve 6. Observe the pressure gauge 4 and use the vacuum system to pump the pipeline into an extreme negative pressure state. Then close the fourth ball valve 6 and open the fifth ball valve 7 to replenish nitrogen. Repeat the replacement three times. (3) Keep the first ball valve 2 and the fifth ball valve 7 closed again, and open the second ball valve 3, the third ball valve 5 and the fourth ball valve 6. After the pipeline is pumped to the ultimate negative pressure, close the second ball valve 3, slowly open the first ball valve 2 and observe the sight glass 1 at the same time, until liquid flows into the pipeline, until the pressure gauge 4 has a slight pressure, close the first ball valve 2, slowly open the second ball valve 3, observe the sampling volume, collect a sufficient amount of liquid sample into the sampling bottle, and then close the second ball valve 3; (4) Keep the first ball valve 2 and the third ball valve 5 open. After the pressure is balanced, open the fifth ball valve 7 to back-blow the liquid into the reactor or container. When no liquid flows into the sight glass 1, close the first ball valve 2 and the fifth ball valve 7 at the same time.
[0013] In summary, the above sampling method can effectively prevent diethyl zinc from coming into contact with air or remaining on the pipeline during the sampling process, thereby effectively improving the accuracy of the secondary sampling samples.
[0014] In general, terms should be understood, at least in part, by the context in which they are used. For example, the term "one or more" as used herein may be used to describe any feature, structure, or characteristic in a singular sense, or may be used to describe a combination of features, structures, or characteristics in a plural sense, depending, at least in part, on the context. Similarly, terms such as "a," "an," or "the" may also be understood to convey singular usage or to convey plural usage, depending, at least in part, on the context.
[0015] It should be easily understood that “on,” “above,” and “over” in the present disclosure should be interpreted in the broadest manner, so that “on” not only means “directly on something,” but also includes the meaning of “on something” with intervening features or layers therebetween, and “above” or “over” not only includes the meaning of “above” or “over,” but also may include the meaning of “above” or “over something” with no intervening features or layers therebetween (i.e., directly on something).
[0016] In addition, spatially relative terms, such as "below," "below," "beneath," "above," "above," etc., may be used herein for ease of description to describe the relationship of one element or feature relative to other elements or features as shown in the figures. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation shown in the figures. The device may have other orientations (rotated 90 degrees or at other orientations), and the spatially relative descriptors used herein may likewise be interpreted accordingly.
[0017] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.
Claims
1. A closed sampling system for diethyl zinc, comprising a pipeline for communicating with a reaction kettle or a container, characterized in that: A plurality of ball valves for opening and closing are arranged at intervals on the upper part of the pipeline. A conical flask for sampling operation is threadedly connected to the upper part of the pipeline. One end of the pipeline is connected to the vacuum system, and the other end of the pipeline is connected to the reactor or container. A nitrogen inlet for blowing nitrogen is also arranged at one end of the upper part of the pipeline close to the vacuum system.
2. A closed sampling system suitable for diethyl zinc according to claim 1, characterized in that: A pressure gauge is also added to the upper part of the pipeline to monitor the pressure inside the pipe.
3. A closed sampling system suitable for diethyl zinc according to claim 2, characterized in that: The number of the ball valves is five, which are sequentially divided into a first ball valve, a second ball valve, a third ball valve, a fourth ball valve and a fifth ball valve.
4. A closed sampling system suitable for diethyl zinc according to claim 3, characterized in that: The first ball valve is arranged at the upper part of the pipeline between the sight glass and the pressure gauge, the second ball valve is arranged at the upper part of the pipeline between the first ball valve and the conical flask, the third ball valve is arranged at the upper part of the pipeline close to the pressure gauge, the fourth ball valve is arranged at the upper part of the pipeline close to the vacuum system, and the fifth ball valve is arranged at the upper part of the pipeline close to the nitrogen inlet.
5. A sampling method, based on the closed sampling system according to claim 4, characterized in that: Here are the steps: (1) Toluene solution is pre-added to a sampling conical flask and weighed. The conical flask is connected to the pipeline via a thread; (2) Keep the first and fifth ball valves closed, and open the second, third and fourth ball valves. Observe the pressure gauge and use the vacuum system to pump the pipeline into an extreme negative pressure state. Then close the fourth ball valve and open the fifth ball valve to replenish nitrogen. Repeat the replacement three times. (3) Keep the first ball valve and the fifth ball valve closed again, and open the second ball valve, the third ball valve and the fourth ball valve. After the pipeline is pumped to the ultimate negative pressure, close the second ball valve, slowly open the first ball valve and observe the sight glass at the same time until liquid flows into the pipeline and until there is a slight pressure on the pressure gauge. Close the first ball valve, slowly open the second ball valve, observe the sampling volume, collect a sufficient amount of liquid sample into the sampling bottle, and then close the second ball valve; (4) Keep the first and third ball valves open. After the pressure is balanced, open the fifth ball valve to backflush the liquid into the reactor or container. When no liquid flows into the sight glass, close the first and fifth ball valves at the same time.