Sampling device based on ethyl chloroacetate and intermediate product mixture

Abstract

The utility model relates to the technical field of related sampling in an ethyl chloroacetate synthesis process, in particular to a sampling device based on ethyl chloroacetate and an intermediate product mixture, which comprises a plurality of sample storage units arranged at intervals, the bottom of each sample storage unit is detachably mounted in a bottom restraint unit below the sample storage unit, and the sample storage units are connected with the sample storage units. A sampling drainage unit is arranged above each sample storage unit, the inlet end of each sampling drainage unit is connected with a sampling port of an upstream chemical reaction kettle, and the inside of the chemical reaction kettle is used for storing raw materials and intermediate products for synthesizing ethyl chloroacetate. The sampling device is mainly used for sampling a mixture of an intermediate product and an internal original solution in the reaction process of ethyl chloroacetate in the synthesis process of ethyl chloroacetate, and can be directly mounted at a chemical reaction degree sampling port in a matched manner, and the mixture can be quickly sampled as required by directly utilizing a metering pump during sampling; and the sampling accuracy is ensured.

Description

TECHNICAL FIELD

[0001] The utility model relates to the sampling technology field related in the chloroacetic acid ethyl ester synthesis process especially based on the sampling device of chloroacetic acid ethyl ester and intermediate product mixture. BACKGROUND

[0002] Chloroacetic acid ethyl ester is an organic compound, which is mainly used as a solvent and can also be used for organic synthesis. In the process of synthesizing chloroacetic acid ethyl ester, a series of chemical reactions are usually involved, which may produce different intermediate products.

[0003] At present, in the production workshop, it is necessary to analyze the current reaction process according to the different synthesis paths and the specific residues of intermediate products. In the prior art, the detection and analysis of the relevant components of part of the chloroacetic acid ethyl ester and intermediate product mixture are mainly realized by the way of sampling inside the reaction kettle.

[0004] Through retrieval, in the patent literature with patent application number CN201822232887.3, a sampling device for chemical synthesis is disclosed, which mainly includes a sampling box body, a foot pad, a top cover, a lock, a controller, a sampling pipe, a main control valve, a sampling pump, a flow guide pipe, a first sample storage bottle, a second sample storage bottle, a third sample storage bottle, a cleaning liquid storage box body and other key components.

[0005] As can be seen, when working, it mainly completes the sampling and placing operation of a plurality of different chemical synthesis reagents in turn by setting the first sample storage bottle, the second sample storage bottle and the third sample storage bottle, and improves the sampling range of the sampling device. However, when cooperating with the subsequent sampling detection operation, the following problems exist:

[0006] Firstly, the above-mentioned sampling device mainly adopts the way of arranging a plurality of sample storage bottles in parallel to complete the sample storage and sampling action. When it is necessary to directly detect and analyze the internal sample on site, it is not convenient to take out each sample storage bottle one by one and perform titration and other operations.

[0007] Secondly, when the sample in a certain sample storage bottle needs to be analyzed, it is necessary to frequently open and close the sample storage bottle to complete the pouring of the sample in batches, which also increases the complexity of the operation steps.

[0008] Based on this, the utility model analyzes the sample sampling problem in chemical synthesis in the prior art and proposes a sampling device suitable for chloroacetic acid ethyl ester and intermediate product mixture to better solve the problems existing in the prior art. INVENTION CONTENTS

[0009] The utility model discloses a technical scheme that is adopted for solving one of the above technical problems: a sampling device based on ethyl chloroacetate and intermediate product mixture, comprising a plurality of interval arranged sample storage units, the bottom of each sample storage unit is detachably installed in the bottom restraint unit below, a sampling drainage unit is arranged above each sample storage unit, the inlet end of the sampling drainage unit is connected with the sampling port of the upstream chemical reaction kettle, the chemical reaction kettle is used for storing raw materials and intermediate products for synthesizing ethyl chloroacetate, and each outlet end of the sampling drainage unit is communicated with the top of the corresponding sample storage unit below.

[0010] Preferably in any of the above solutions, the sampling drainage unit comprises a drainage pipe with a metering pump, the inlet end of the drainage pipe is connected with the sampling port of the upstream chemical reaction kettle through a connecting joint, a multi-way pipeline is connected to the end of the drainage pipe, a blocking cap is installed on the outer side wall of the pipe opening of each branch pipeline of the multi-way pipeline, a blocking cavity with an open bottom is arranged in each blocking cap, each blocking cavity is used for sleeving the top outer side wall of the sample storage unit below, and the lower end of each branch pipeline extends into the corresponding sample storage unit.

[0011] Preferably in any of the above solutions, the sample storage unit comprises a vertically arranged sample storage bottle, a sample storage cavity is arranged in the sample storage bottle, a sample inlet for the branch pipeline is arranged on the top of the sample storage bottle, and the lower part of each sample storage bottle is inserted into the bottom restraint unit.

[0012] Preferably in any of the above solutions, a branch flow valve is installed on each branch pipeline.

[0013] Preferably in any of the above solutions, the bottom restraint unit comprises a fixedly arranged mounting seat, a restraint seat is fixed on the top of the mounting seat, a plurality of mounting spaces are arranged on the top of each restraint seat at intervals, a plurality of supporting springs are fixedly installed on the bottom of each mounting space, a restraint sleeve is arranged in the mounting space above each supporting spring, the bottom of the restraint sleeve is fixed on the top of each supporting spring, a limiting cavity is arranged on the top of each restraint sleeve, each limiting cavity is used for movably sleeving the lower outer side wall of the sample storage bottle, and each supporting spring can be compressed downward when the sample storage bottle is pressed downward.

[0014] Preferably in any of the above solutions, a sampling valve is arranged on the lower outer side wall of each sample storage bottle.

[0015] Preferably in any of the above solutions, the upper part of the sample storage bottle is provided with a bottle neck, a lower magnet is fixedly installed on the top of the shaft shoulder end face of the bottle neck, an upper magnet is arranged on the top step surface of the shielding cavity, and the upper magnet and the lower magnet are attracted to each other and abut against each other.

[0016] Preferably in any of the above solutions, the front and rear ends of each installation space are open.

[0017] Compared with the prior art, the utility model has the beneficial effects as follows:

[0018] 1. The sampling device in the utility model is mainly used for sampling the mixture of intermediate products and original solutions in the reaction process of ethyl chloroacetate synthesis, and can be directly installed at the sampling port of a chemical reaction device, so that the mixture can be quickly sampled on demand by using a metering pump during sampling, and the accuracy of sampling is ensured.

[0019] 2. The sample storage unit designed in the utility model can sample in cooperation with the sampling and drainage unit above, and can complete sampling on demand under the action of the flow valves on each branch pipeline; the multiple sampling bottles arranged can complete sampling and storage of the mixture under different reaction durations, so as to facilitate downstream detection and analysis to achieve the purpose of judging the internal reaction effect under different reaction durations.

[0020] 3. The top of each sample storage bottle is fixed by magnetic attraction to achieve upper positioning, and the bottom is limited by the bottom limiting unit, so that when it is necessary to remove the sample storage bottle outward, the operator can press the entire sample storage bottle downward, so as to move downward and overcome the elastic force of the supporting spring, so that the upper part of the sample storage bottle is separated from the shielding cavity, and then the sample storage bottle can be removed from the inside of the bottom limiting unit by tilting forward or backward, so as to quickly replace the corresponding empty sample storage bottle, which is convenient and fast.

[0021] 4. When the sample storage bottle is normally installed, the upward support of the bottom supporting spring and the magnetic attraction of the upper part of each sample storage bottle can better ensure the stability of the positioning of the entire sample storage bottle. BRIEF DESCRIPTION OF DRAWINGS

[0022] In order to more clearly illustrate the specific embodiments of the utility model or the technical solutions in the prior art, the drawings needed in the specific embodiments or the prior art description will be briefly introduced below. In all the drawings, similar elements or components are generally identified by similar reference numerals. In the drawings, each element or component is not necessarily drawn according to the actual scale.

[0023] Figure 1 It is a structural schematic view of the sampling device of the utility model.

[0024] Figure 2 It is the internal structure schematic view of the sampling device of the utility model.

[0025] Figure 3 It is the structure schematic view of the sample storage bottle of the utility model.

[0026] Figure 4 It is the internal structure schematic view of the bottom restraint unit of the utility model.

[0027] In the figure, 1, drainage tube;2, metering pump;3, multi-way pipeline;301, branch pipeline;4, shielding cap;401, shielding cavity;5, sample storage bottle;501, bottle neck part;502, lower magnet;503, upper magnet;6, sample storage cavity;7, branch flow valve;8, mounting seat;9, restraint seat;10, mounting space;11, sampling valve;12, supporting spring;13, restraint sleeve;14, limiting cavity. DETAILED DESCRIPTION

[0028] The embodiments of the technical scheme of the utility model will be described in detail below with reference to the drawings. The following embodiments are only used to more clearly illustrate the technical scheme of the utility model, therefore only as an example, and cannot limit the protection scope of the utility model. The specific structure of the utility model is shown in Figures 1-4

[0029] Embodiment 1: the sampling device based on ethyl chloroacetate and intermediate product mixture, including several interval arrangement's sample storage unit, the bottom of each sample storage unit is detachably installed in the bottom restraint unit below, the sampling drainage unit is arranged above each sample storage unit, the inlet end of the sampling drainage unit is connected with the sampling port of the upstream chemical reaction kettle, the chemical reaction kettle is used to store the raw materials and intermediate products for synthesizing ethyl chloroacetate, and each outlet end of the sampling drainage unit is communicated with the top of the corresponding sample storage unit below.

[0030] It should be noted that: the sampling device in the utility model needs to be installed and positioned according to the needs before use, the bottom of the bottom restraint unit is fixed during positioning, at the same time, the sampling drainage unit remains fixed after being installed with the external chemical reaction kettle, at this time, the corresponding sample storage unit is installed in the inside of the bottom restraint unit according to the needs, the bottom of the sample storage unit is completed to be pressed upward by the supporting spring 12 after the installation of the sample storage unit is completed, the restraint positioning of the upper part of the sample storage unit is completed by the magnetic attraction fixation of the lower magnet 502 and the upper magnet 503 in the upper part of the sample storage unit, the comprehensive positioning effect can be effectively achieved by the spring abutting and the upper magnetic attraction restraint positioning, and the fixing effect of the whole sample storage unit after installation is ensured.

[0031] ​Preferably in any of the above solutions, the sampling drainage unit comprises a drainage pipe 1 with a metering pump 2, the inlet end of the drainage pipe 1 is connected with the sampling port of the upstream chemical reaction kettle through a connecting joint 101, a multi-way pipe 3 is connected at the end of the drainage pipe 1, a shielding cap 4 is respectively installed on the outer wall of the pipe opening of each branch pipe 301 of the multi-way pipe 3, an open-bottom shielding cavity 401 is arranged in each shielding cap 4, each shielding cavity 401 is used for sleeving on the top outer wall of the corresponding sampling storage unit below, and the lower end of each branch pipe 301 extends into the inside of the corresponding sampling storage unit.

[0032] The sampling drainage unit is installed at the sampling port of the chemical reaction kettle through the drainage pipe 1, and the relative fixation of the drainage pipe 1 is maintained after installation. At this time, each branch pipe 301 of the multi-way pipe 3 at the end of the drainage pipe 1 can be matched and connected with each sampling storage unit below, respectively. When connected, the shielding cap 4 is directly covered on the upper outer wall of the bottle neck part 501 of the sampling bottle 5 of the corresponding sampling storage unit, so as to circumferentially constrain and position it, so as to ensure that the upper part will not shake left and right, and ensure the relative fixation of the sampling bottle 5 when sampling.

[0033] Preferably in any of the above solutions, the sampling storage unit comprises a vertically arranged sampling bottle 5, the inside of the sampling bottle 5 is provided with a sampling cavity 6, the top of the sampling bottle 5 is provided with a sampling inlet for the branch pipe 301, and the lower part of each sampling bottle 5 is inserted and fitted in the bottom constraint unit.

[0034] The sampling bottle 5 is a container made of transparent glass material, and the sampling cavity 6 in the inside of the sampling bottle 5 can better store the mixture entering the inside, and facilitate the observation of the internal sampling from the outside.

[0035] Preferably in any of the above solutions, a branch flow valve 7 is installed on each branch pipe 301.

[0036] When it is necessary to control the branch pipe 301 to deliver the sampling liquid to the sampling inlet of the sampling bottle 5 below, the branch flow valve 7 can be controlled to achieve the purpose of controlling the sampling speed.

[0037] Preferably in any of the above solutions, the bottom constraint unit comprises a fixedly arranged mounting base 8, a constraint seat 9 is fixedly arranged on the top of the mounting base 8, a plurality of mounting spaces 10 are arranged on the top of each constraint seat 9, a plurality of supporting springs 12 are fixedly arranged on the bottom of each mounting space 10, a constraint sleeve 13 is arranged in each mounting space 10 above each supporting spring 12, the bottom of the constraint sleeve 13 is fixedly arranged on the top of each supporting spring 12, a limiting cavity 14 is arranged on the top of each constraint sleeve 13, and each limiting cavity 14 is movably sleeved on the lower outer sidewall of the sample storage bottle 5 and can drive each supporting spring 12 to compress downward when the sample storage bottle 5 is pressed downward.

[0038] The whole structure of the bottom constraint unit is positioned by the mounting base 8 at the bottom, and the mounting base 8 is bolted and fixed when installation is required. Since the two ends of each constraint seat 9 arranged on the top are both arranged in an open manner, each supporting spring 12 can be inclined forward and backward in the mounting space 10, so that the constraint sleeve 13 connected thereto can be inclined and positioned as required.

[0039] Embodiment 2: Compared with Embodiment 1, the difference lies in that it further comprises the following technical features:

[0040] Preferably in any of the above solutions, a sampling valve 11 is arranged on the lower outer sidewall of each sample storage bottle 5.

[0041] After the mixed solution formed by the ethyl chloroacetate and the intermediate product mixture is loaded in the sample storage bottle 5, the opening and closing of the sampling valve 11 can be controlled to transfer the mixed solution to the container outside as required, so as to achieve the purpose of rapid sampling for small sample analysis. This operation can realize multiple intermittent sampling, and the sample in the sample storage bottle 5 will not be contaminated.

[0042] Preferably in any of the above solutions, the upper part of the sample storage bottle 5 is provided with a neck portion 501, a lower magnet 502 is fixedly arranged on the top of the shaft shoulder end face of the neck portion 501, and an upper magnet 503 is arranged on the top stepped surface of the shielding cavity 401, and the upper magnet 503 and the lower magnet 502 are arranged in close contact with each other by mutual attraction.

[0043] Considering the relative stability of the upper part of the sample storage bottle 5 after being sleeved in the corresponding shielding cavity 401, the corresponding lower magnet 502 and upper magnet 503 are additionally arranged to realize mutual magnetic attraction and fixation, which not only ensures the constraint and positioning of the sample storage bottle 5 in the circumferential direction, but also ensures that the sample storage bottle 5 can block the downward displacement together with the supporting spring 12 below, thereby ensuring the relative stability of the sample storage bottle 5 after installation.

[0044] In any of the above schemes, preferably, the front and rear ends of each mounting space 10 are open. Considering that the top of the restraint seat 9 is provided with two ends of each open structure, the support spring 12 can be tilted forward and backward inside the mounting space 10, so that the restraint sleeve 13 connected thereto can be tilted and positioned as needed, and the lower part of each sample bottle 5 can be pressed and tilted to quickly pull out the sample bottle 5.

[0045] Specific working principle: Before use, the entire structure needs to be installed and positioned as needed. When positioning, the bottom of the bottom restraint unit is fixed, and the sampling drainage unit is fixed after being installed with the external chemical reaction kettle. At this time, the corresponding sample storage unit is installed in the bottom restraint unit as needed, and the bottom of the sample storage unit is pressed upward by the support spring 12 after installation is completed.

[0046] The upper part of the sample storage unit is fixed and positioned by the magnetic attraction of the lower magnet 502 and the upper magnet 503 on the upper part of the sample storage unit. The spring abutting and the magnetic attraction positioning of the upper part can effectively play a comprehensive positioning role, ensuring the fixing effect of the entire sample storage unit after installation is completed.

[0047] When the sample bottle 5 is filled with a mixture of ethyl chloroacetate and intermediate product mixture to form a mixed liquid, the opening and closing of the sampling valve 11 can be controlled to transfer it to the outside container as needed, so as to achieve the purpose of rapid sampling for small sample analysis. This operation can realize multiple intermittent sampling, without worrying about the contamination of the sample mixture in the sample bottle 5. When the corresponding branch pipeline 301 is used to transport the sampling liquid to the sample inlet of the sample bottle 5 below, the branch flow valve 7 can be controlled to control the sampling speed. In addition, after sampling is completed, in order to facilitate subsequent secondary sampling, when the sample bottle 5 is filled with a mixture of ethyl chloroacetate and intermediate product mixture to form a mixed liquid, the opening and closing of the sampling valve 11 can be controlled to transfer it to the outside container as needed, so as to achieve the purpose of rapid sampling for small sample analysis. This operation can realize multiple intermittent sampling, without worrying about the contamination of the sample mixture in the sample bottle 5.

[0048] In summary, the sampling device is mainly used for sampling the mixture of intermediate products and original solution in the reaction process of ethyl chloroacetate synthesis. It can be directly installed at the sampling port of the chemical reaction device. When sampling, the metering pump 2 is used to complete the rapid sampling of the mixture according to the demand, ensuring the accuracy of the sampling. The sample storage unit can cooperate with the sampling drainage unit above to sample, and complete the sampling according to the demand under the action of the flow valve on each branch pipeline 301. The multiple sampling bottles arranged can complete the sampling of the mixture under different reaction times, which is convenient for downstream detection and analysis to judge the internal reaction effect under different reaction times. The top of each sample storage bottle 5 is magnetically fixed to realize upper positioning, and the bottom is limited by the bottom limiting unit. When it is necessary to remove the sample storage bottle 5 outward, the operator can press the whole sample storage bottle 5 downward to make it move downward and overcome the elastic force of the supporting spring 12, so that the upper part of the sample storage bottle 5 is separated from the shielding cavity 401. At this time, tilting forward or backward can remove it from the inside of the bottom limiting unit, which is convenient for quickly replacing the corresponding empty sample storage bottle 5, and the operation is quick and convenient. When the sample storage bottle 5 is normally installed, the upward support of the bottom supporting spring 12 and the magnetic attraction of the upper part of each sample storage bottle 5 can better ensure the stability of the positioning of the whole sample storage bottle 5.

[0049] The above embodiments are only used to illustrate the technical solutions of the present application, but not to limit them. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent substitutions for part or all of the technical features. These modifications or substitutions do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application. Any alternative improvement or change made by those skilled in the art to the embodiments of the present application falls within the scope of protection of the present application.

[0050] The details not described in the present application are well-known to those skilled in the art.

Claims

1. A sampling device based on a mixture of ethyl chloroacetate and intermediate products, characterized in that: The device includes several spaced-apart sample storage units, each of which is detachably mounted at the bottom within a bottom constraint unit below it. A sampling and diversion unit is provided above each of the sample storage units. The inlet of the sampling and diversion unit is connected to the sampling port of an upstream chemical reactor. The chemical reactor is used to store raw materials and intermediate products for the synthesis of ethyl chloroacetate. Each outlet of the sampling and diversion unit is connected to the top of the corresponding sample storage unit below it.

2. The sampling device based on the mixture of ethyl chloroacetate and intermediate products according to claim 1, characterized in that: The sampling and diversion unit includes a diversion pipe with a metering pump. The inlet end of the diversion pipe is connected to the sampling port of the upstream chemical reactor via a connecting joint. A multi-port pipeline is connected to the end of the diversion pipe. A shielding cap is installed on the outer wall of the outlet of each branch pipeline of the multi-port pipeline. Each shielding cap has a shielding cavity with an open bottom. Each shielding cavity is used to fit onto the top outer wall of the corresponding sample storage unit below it. The lower end of each branch pipeline extends into the interior of the corresponding sample storage unit.

3. The sampling device based on the mixture of ethyl chloroacetate and intermediate products according to claim 2, characterized in that: The sample storage unit includes vertically arranged sample bottles, each with a sample storage cavity inside. The top of each sample bottle has an inlet for the branch pipeline to enter, and the lower part of each sample bottle is fitted into the bottom constraint unit.

4. The sampling device based on the mixture of ethyl chloroacetate and intermediate products according to claim 3, characterized in that: Each of the branch pipelines is equipped with a branch flow valve.

5. The sampling device based on the mixture of ethyl chloroacetate and intermediate products according to claim 4, characterized in that: The bottom constraint unit includes a fixed mounting base, a constraint seat fixed on the top of the mounting base, and several mounting spaces spaced apart on the top of each constraint seat. Several support springs are fixedly installed at the bottom of each mounting space. A constraint sleeve is provided in the mounting space above each support spring. The bottom of the constraint sleeve is fixed to the top of each support spring. A limiting cavity is provided on the top of each constraint sleeve. Each limiting cavity is used to movably fit onto the lower outer wall of the sample bottle. When the sample bottle is pressed down, it can drive each support spring to compress downward.

6. The sampling device based on the mixture of ethyl chloroacetate and intermediate products according to claim 5, characterized in that: Each of the aforementioned sample storage bottles is provided with a sampling valve on its lower outer side wall.

7. The sampling device based on a mixture of ethyl chloroacetate and intermediate products according to claim 6, characterized in that: The upper part of the sample storage bottle is provided with a neck section, and a lower magnet is fixedly installed on the top of the shoulder end face of the neck section. An upper magnet is provided on the top stepped surface of the shielding cavity. The upper magnet and the lower magnet attract each other and are pressed against each other.

8. The sampling device based on a mixture of ethyl chloroacetate and intermediate products according to claim 7, characterized in that: Both the front and rear ends of each installation space are open.

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