CN216559892U - Reaction device capable of dynamically and hermetically sampling - Google Patents
Reaction device capable of dynamically and hermetically sampling Download PDFInfo
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- CN216559892U CN216559892U CN202123195249.7U CN202123195249U CN216559892U CN 216559892 U CN216559892 U CN 216559892U CN 202123195249 U CN202123195249 U CN 202123195249U CN 216559892 U CN216559892 U CN 216559892U
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- 238000005070 sampling Methods 0.000 title claims abstract description 95
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 55
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 16
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 239000000523 sample Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000000376 reactant Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- IXVMHGVQKLDRKH-VRESXRICSA-N Brassinolide Natural products O=C1OC[C@@H]2[C@@H]3[C@@](C)([C@H]([C@@H]([C@@H](O)[C@H](O)[C@H](C(C)C)C)C)CC3)CC[C@@H]2[C@]2(C)[C@@H]1C[C@H](O)[C@H](O)C2 IXVMHGVQKLDRKH-VRESXRICSA-N 0.000 description 2
- 239000005497 Clethodim Substances 0.000 description 2
- 239000005931 Spirotetramat Substances 0.000 description 2
- IXVMHGVQKLDRKH-KNBKMWSGSA-N brassinolide Chemical compound C1OC(=O)[C@H]2C[C@H](O)[C@H](O)C[C@]2(C)[C@H]2CC[C@]3(C)[C@@H]([C@H](C)[C@@H](O)[C@H](O)[C@@H](C)C(C)C)CC[C@H]3[C@@H]21 IXVMHGVQKLDRKH-KNBKMWSGSA-N 0.000 description 2
- SILSDTWXNBZOGF-JWGBMQLESA-N clethodim Chemical compound CCSC(C)CC1CC(O)=C(C(CC)=NOC\C=C\Cl)C(=O)C1 SILSDTWXNBZOGF-JWGBMQLESA-N 0.000 description 2
- CLSVJBIHYWPGQY-GGYDESQDSA-N spirotetramat Chemical compound CCOC(=O)OC1=C(C=2C(=CC=C(C)C=2)C)C(=O)N[C@@]11CC[C@H](OC)CC1 CLSVJBIHYWPGQY-GGYDESQDSA-N 0.000 description 2
- 239000005740 Boscalid Substances 0.000 description 1
- 239000005583 Metribuzin Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- WYEMLYFITZORAB-UHFFFAOYSA-N boscalid Chemical compound C1=CC(Cl)=CC=C1C1=CC=CC=C1NC(=O)C1=CC=CN=C1Cl WYEMLYFITZORAB-UHFFFAOYSA-N 0.000 description 1
- 229940118790 boscalid Drugs 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000005574 cross-species transmission Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000004495 emulsifiable concentrate Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- FOXFZRUHNHCZPX-UHFFFAOYSA-N metribuzin Chemical compound CSC1=NN=C(C(C)(C)C)C(=O)N1N FOXFZRUHNHCZPX-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- IYMLUHWAJFXAQP-UHFFFAOYSA-N topramezone Chemical compound CC1=C(C(=O)C2=C(N(C)N=C2)O)C=CC(S(C)(=O)=O)=C1C1=NOCC1 IYMLUHWAJFXAQP-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The application relates to a reaction device capable of dynamically and hermetically sampling, which comprises (i) a reaction kettle; (ii) a circulating valve arranged at the bottom of the reaction kettle; (iii) an inlet of the circulating pump is connected with the circulating valve through an upstream circulating pipeline, and an outlet of the circulating pump is connected with the top of the reaction kettle through a downstream circulating pipeline; and (iv) a sampling bin which is arranged on the downstream circulating pipeline and is close to the position of a connecting port between the circulating pipeline and the top of the reaction kettle, the top of the sampling bin is connected with the downstream circulating pipeline through a sampling pipeline, the sampling pipeline extends into the sampling bin, a sampling valve is arranged at a pipeline outlet positioned in the sampling bin, a tail gas pipeline with a tail gas valve is also arranged at the top of the sampling bin, the bottom of the sampling bin is connected with the top of the reaction kettle through a discharging pipeline with a discharging valve, a bin gate capable of being opened and closed is arranged on the front side of the sampling bin, and the lower edge of the bin gate is higher than the bottom of the sampling bin.
Description
Technical Field
The application relates to a reaction device capable of dynamically and hermetically sampling.
Background
In chemical industry production, often need follow reation kettle sample, open reation kettle manhole or the valve on the reation kettle, then take a sample with the vial, such open sampling operation can lead to the gas in the reation kettle to spill over and cause gaseous inorganization to discharge, not only cause the atmospheric pollution, still bring harmful effects to operator's health. Moreover, the sampling of the small bottle easily causes the spilling of reactants, which causes the waste of materials and the environmental pollution.
In addition, when the pH value of the reactant needs to be monitored in some reactions, the pH meter is usually fixed in the reaction kettle, and the probe of the pH meter extends below the liquid level of the reactant, so that when the liquid level of the reactant is lower than the probe of the pH meter, the pH value of the reactant can not be monitored any more, which is not favorable for stable monitoring of the reaction and is easy to cause reaction accidents. In addition, the glass bulb of the pH meter is exposed in the reaction kettle for a long time and is not maintained in time, so that the service life of the pH meter is easily shortened.
SUMMERY OF THE UTILITY MODEL
An object of this application is to provide a reaction unit that can developments airtight sample, through carry out the sample operation in the sample storehouse airtight relatively, can solve the problem that the gas unorganized emission and material spilled in the current open sample operation.
Further, when the reaction device capable of dynamically and hermetically sampling is used for reaction or material treatment needing monitoring of the pH value, a pH meter is preferably further arranged in the reaction device to monitor the pH value of materials in the reaction kettle in real time, and the pH value of the materials can be stably monitored by the aid of the arrangement, so that accidents caused by the fact that the monitoring cannot be conducted due to too low liquid level and further accidents are avoided.
In particular, the present application relates to:
(1) reaction device capable of dynamic closed sampling, characterized in that it comprises: (i) a reaction kettle; (ii) a circulating valve arranged at the bottom of the reaction kettle; (iii) the inlet of the circulating pump is connected with the circulating valve through an upstream circulating pipeline, and the outlet of the circulating pump is connected with the top of the reaction kettle through a downstream circulating pipeline; and (iv) a sampling bin, wherein the sampling bin is arranged on the downstream circulating pipeline at a position close to a connecting port of the circulating pipeline and the top of the reaction kettle, the top of the sampling bin is connected with the downstream circulating pipeline through a sampling pipeline, the sampling pipeline extends into the sampling bin, a sampling valve is arranged at a pipeline outlet positioned in the sampling bin, a tail gas pipeline with a tail gas valve is further arranged at the top of the sampling bin, the bottom of the sampling bin is connected with the top of the reaction kettle through a discharging pipeline with a discharging valve, a bin gate capable of being opened and closed is arranged on the front side of the sampling bin, and the lower edge of the bin gate is higher than the bottom of the sampling bin.
(2) The reaction apparatus according to the above (1), wherein a pH meter is provided on the upstream or downstream circulation line.
(3) The reaction apparatus according to the above (2), wherein the pH meter is fixed to the upstream or downstream circulation line by a screw thread.
(4) The reaction apparatus according to any one of the above (1) to (3), wherein the sampling well has a rectangular parallelepiped shape.
(5) The reaction apparatus according to any one of the above (1) to (4), wherein the upstream circulation line length is smaller than the downstream circulation line length.
(6) The reaction apparatus according to any one of the above (1) to (5), wherein the lower edge of the chamber door is higher than the bottom of the sampling chamber by 1cm or more.
Drawings
FIG. 1 is a schematic structural diagram of a preferred embodiment of the present invention, which is a reaction apparatus capable of dynamic closed sampling.
Fig. 2 is a schematic perspective view of a preferred embodiment of a sampling chamber.
Description of reference numerals:
1: a reaction kettle; 2: a circulation valve; 3: an upstream circulation line; 4: a circulation pump; 5: a downstream circulation line; 6: sampling a bin; 7: a sampling pipeline; 8: a sampling valve; 9: a tail gas valve; 10: a discharge pipeline; 11: a discharge valve; 12: threading; 13: a bin gate.
Detailed Description
The preferred structure of the reactor apparatus for dynamic closed sampling according to the present invention will be described in more detail with reference to the accompanying drawings, but the present invention is not limited to the specific embodiment, and any modification and variation within the scope of the present invention will fall within the scope of the present invention.
The reaction device capable of dynamically and hermetically sampling comprises a reaction kettle 1, a sampling bin 6 and a connecting part between the reaction kettle 1 and the sampling bin.
In this application, reaction vessel 1 has a broad meaning, and includes a reaction vessel for preparing a raw material drug by a chemical reaction, a reaction vessel for processing the raw material drug and an auxiliary material into a preparation, and a pretreatment vessel for pretreating a reaction raw material. The kettle body structure and the accessories thereof can adopt the known structures and accessories according to the purposes, for example, a stirrer is assembled when the materials need to be stirred, and a cold or hot medium jacket is assembled when the temperature needs to be controlled, etc.
A circulating pipeline is led out from the bottom of the reaction kettle 1 and communicated to the top of the reaction kettle, and a circulating valve 2 and a circulating pump 4 are arranged on the circulating pipeline. The part between the kettle bottom and the circulating pump 4 is an upstream circulating pipeline 3, and the part between the circulating pump 4 and the kettle top is a downstream circulating pipeline 5. The circulating valve 2 is arranged near the bottom of the reaction kettle 1, and the position of the circulating valve is determined according to the convenience of valve switching operation. The length ratio of the upstream circulation line 3 to the downstream circulation line 5 is not particularly limited, but it is generally preferable that the upstream section is shorter than the downstream section in view of the pipe resistance.
The sampling bin 6 is arranged on the downstream circulation line 5 at a position close to the connection of the circulation line and the top of the reaction vessel 1. The top of the sampling bin 6 is connected with the downstream circulating pipeline 5 through a sampling pipeline 7, and the sampling pipeline 7 extends into the sampling bin 6. A sampling valve 8 is arranged at the outlet of the sampling pipeline 7 positioned inside the sampling bin 6.
The top of sampling storehouse 6 still sets up the tail gas pipeline that has tail gas valve 9, and this tail gas pipeline is connected with the tail gas pipeline of mill, and the gaseous inorganization when preventing to take a sample is discharged.
The bottom of the sampling bin 6 is connected with the top of the reaction kettle 1 through a discharging pipeline 10 with a discharging valve 11. The sampling pipeline 7 and the discharging pipeline 10 have the functions of fixing and supporting the sampling bin 6.
An openable and closable bin gate 13 is provided on the front surface of the sampling bin 6. The door 13 is opened when sampling and closed when not sampling. The lower edge of the bin gate 13 is higher than the bottom of the sampling bin 6, so as to prevent liquid overflowing and discharging during sampling from spilling on the ground, and the higher height only needs to be enough to block the liquid from overflowing and discharging from the bin and not to prevent a small bottle manually held from extending into the sampling bin 6 to open the valve for sampling. In general, the amount of liquid overflowing during sampling is not large, and therefore the lower edge of the bin gate 13 is preferably higher than the bottom of the sampling bin 6 by more than 1 cm.
The sampling bin 6 can be any shape which is convenient for a person to manually hold a small bottle to extend into the sampling bin to open a valve for sampling, and is preferably in a cuboid shape, the size of the sampling bin can be as long as the requirement of convenience in sampling operation can be met, the length, the width and the height of the sampling bin are respectively 10-30 cm, and a cuboid with the length of 20cm multiplied by the width of 10cm multiplied by the height of 10cm can be listed.
When the pH value of the material needs to be monitored, a pH meter can be arranged on the upstream circulating pipeline 3 or the downstream circulating pipeline 5, and the specific position is convenient for observation. It is preferable to weld the screw 12 at any position of the upstream or downstream circulation line and then screw the pH meter with the screw 12, thereby fixing the pH meter on the upstream or downstream circulation line.
When a sample is needed, the circulating valve 2 and the circulating pump 4 are opened in advance to circulate the materials, and the circulating pump 4 operates for 10-20 minutes, preferably for about 15-20 minutes to ensure that the materials in the reaction kettle 1 are circulated to form a uniform composition. At the moment, the bin gate 13 and the tail gas valve 9 are opened, then the small bottle is taken into the sampling bin 6, and the sampling valve 8 is opened to manually receive the sample. After sampling, the sampling valve 8, the circulating valve 2 and the circulating pump 4 are closed, then the discharging valve 11 is opened to enable materials overflowing during sampling to return to the reaction kettle 1 through the discharging pipeline 10, and finally the bin gate 13 and the tail gas valve 9 are closed.
When the pH value needs to be monitored, the circulating valve 2 and the circulating pump 4 are also opened in advance to ensure that the materials are circulated to form uniform components, and then the pH value is measured.
When sampling and pH value monitoring are needed, the sampling and pH value measurement operations are carried out simultaneously or sequentially.
Through the device of this application, can carry out dynamic sampling and monitoring as above, the sample composition that the sample that dynamic sampling obtained after making the material fully circulate is more even than the sample that static sampling obtained, therefore the testing result is more accurate. Simultaneously, as mentioned above, through setting up the sample storehouse 6 that has the tail gas pipeline, gaseous inorganization emission when can avoid taking a sample to, bin gate 13 is lower along the structure that is higher than the 6 bottoms in sample storehouse makes the material of the overflow ejection of compact can not spill to the outside and store up in the storehouse bottom, open the blowing valve 11 back flow back to reation kettle when taking a sample in, avoid extravagant and pollution.
The application of the device of the present invention may be preferably applied to the preparation of bulk drugs such as clethodim, topramezone, spirotetramat, brassinolide, boscalid, metribuzin, the preparation of emulsifiable concentrate formulations of clethodim, the preparation of suspending agents of spirotetramat, the preparation of aqueous solutions of brassinolide, and the pretreatment of raw materials in the above preparation, but the present invention is not limited thereto.
Industrial applicability
The device can realize the pH value of airtight dynamic sampling and real-time monitoring materials, can well solve the problem that gas is discharged in an unorganized mode in the sampling process and the pH value when the liquid level of the reaction liquid is lower than a pH meter probe cannot be monitored, and has high industrial application value.
Claims (6)
1. Reaction device capable of dynamic closed sampling, characterized in that it comprises:
(i) a reaction kettle;
(ii) a circulating valve arranged at the bottom of the reaction kettle;
(iii) the inlet of the circulating pump is connected with the circulating valve through an upstream circulating pipeline, and the outlet of the circulating pump is connected with the top of the reaction kettle through a downstream circulating pipeline; and
(iv) the sampling bin is arranged at a position, close to a connecting port of the circulating pipeline and the top of the reaction kettle, on the downstream circulating pipeline, the top of the sampling bin is connected with the downstream circulating pipeline through the sampling pipeline, the sampling pipeline stretches into the sampling bin, a sampling valve is arranged at a pipeline outlet inside the sampling bin, a tail gas pipeline with a tail gas valve is further arranged at the top of the sampling bin, the bottom of the sampling bin is connected with the top of the reaction kettle through a discharging pipeline with a discharging valve, a bin gate capable of being opened and closed is arranged on the front side of the sampling bin, and the lower edge of the bin gate is higher than the bottom of the sampling bin.
2. The reactor apparatus according to claim 1, wherein a pH meter is provided on the upstream or downstream circulation line.
3. The reaction device according to claim 2, wherein the pH meter is fixed to the upstream or downstream circulation line by a screw thread.
4. The reaction device according to any one of claims 1 to 3, wherein the sampling chamber has a rectangular parallelepiped shape.
5. The reactor apparatus as claimed in any one of claims 1 to 3, wherein the upstream circulation line length is smaller than the downstream circulation line length.
6. The reactor according to any one of claims 1 to 3, wherein the lower edge of the bin gate is higher than the bottom of the sampling bin by more than 1 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123195249.7U CN216559892U (en) | 2021-12-20 | 2021-12-20 | Reaction device capable of dynamically and hermetically sampling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123195249.7U CN216559892U (en) | 2021-12-20 | 2021-12-20 | Reaction device capable of dynamically and hermetically sampling |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216559892U true CN216559892U (en) | 2022-05-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202123195249.7U Active CN216559892U (en) | 2021-12-20 | 2021-12-20 | Reaction device capable of dynamically and hermetically sampling |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN216559892U (en) |
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2021
- 2021-12-20 CN CN202123195249.7U patent/CN216559892U/en active Active
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 052260 No.1, Hongsheng Road West, Mayu Village, Mayu Township, Jinzhou City, Shijiazhuang City, Hebei Province Patentee after: Lansheng Biotechnology Group Co.,Ltd. Patentee after: Hebei lanrun Plant Protection Technology Co.,Ltd. Address before: 052260 Mayu village, Jinzhou City, Shijiazhuang City, Hebei Province Patentee before: HEBEI LANSHENG BIOTECH Co.,Ltd. Patentee before: Hebei lanrun Plant Protection Technology Co.,Ltd. |
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| CP03 | Change of name, title or address |