CN219302098U

CN219302098U - Closed digestion device for extracting metal ions of ethyl orthosilicate

Info

Publication number: CN219302098U
Application number: CN202320272706.8U
Authority: CN
Inventors: 徐聪; 杨开乔; 陈琪; 孙猛; 孔超
Original assignee: Jinhong Gas Co ltd
Current assignee: Jinhong Gas Co ltd
Priority date: 2023-02-21
Filing date: 2023-02-21
Publication date: 2023-07-04
Anticipated expiration: 2033-02-21

Abstract

The utility model discloses a closed digestion device for extracting metal ions of ethyl orthosilicate, which comprises a digestion tank. The digestion tank is arranged on a heating device, and the heating device is used for heating the tetraethoxysilane in the digestion tank. The upper wall of the digestion tank is provided with a mixed acid adding pipe and a raw material adding pipe which are respectively used for adding mixed acid and raw materials into the digestion tank. Be equipped with nitrogen gas connecting pipe and vacuum connecting pipe on the lateral wall of digestion tank, nitrogen gas connecting pipe is used for letting in nitrogen gas to digestion tank, and vacuum connecting pipe is used for taking out nitrogen gas and other miscellaneous gas in the digestion tank to digestion tank be negative pressure, and vacuum connecting pipe also is used for taking out the tetraethoxysilane after the digestion. The bottom wall of the digestion tank is provided with an acid liquor discharge pipe which is used for discharging the mixed solution of the mixed oil metal to a designated position, thus the extraction of trace metal ions in the tetraethoxysilane is completed, and the sealed digestion device for extracting the metal ions of the tetraethoxysilane is simple to operate and efficient in treatment.

Description

Closed digestion device for extracting metal ions of ethyl orthosilicate

Technical Field

The utility model relates to the technical field of chemical engineering, in particular to a closed digestion device for extracting metal ions of tetraethoxysilane.

Background

At present, for trace ppb level metal ion detection, an inductively coupled plasma mass spectrometer (ICP-MS) is used for corresponding test, and the detection precision can reach ppt level. However, due to the specificity of TEOS (tetraethyl orthosilicate), it is not possible to test the sample directly into the instrument, since it dissociates a large amount of Si into SiO in the plasma state ₂ Resulting in detector failure.

In the chemical industry, closed digestion tanks are used to dissolve samples under acidic or alkaline conditions by heating and then to extract the desired substances. The existing system is complex in structure, more in pipelines and more in tank bodies, the requirements of ultra-clean rooms cannot be met, and when the system is heated, the temperature needs to reach 130-150 ℃, and for TEOS samples possibly mixed with a small amount of ethanol, the temperature has fire and high-temperature dangers, and the efficiency of experimental operators in preparing the samples for many times and the risk of high-temperature scalding are seriously affected.

The information disclosed in this background section is only for enhancement of understanding of the general background of the utility model and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.

Disclosure of Invention

The utility model aims to provide a closed digestion device for extracting metal ions of ethyl orthosilicate, which can effectively solve the problems of low efficiency and high risk coefficient when extracting metal ions from ethyl orthosilicate.

In order to achieve the above object, the utility model provides a closed digestion device for extracting metal ions of ethyl orthosilicate, which comprises a digestion tank. The digestion tank is arranged on the heating device, the upper wall of the digestion tank is provided with a mixed acid adding pipe and a raw material adding pipe, the side wall of the digestion tank is provided with a nitrogen connecting pipe and a vacuum connecting pipe, and the bottom wall of the digestion tank is provided with an acid liquor discharging pipe.

In one or more embodiments, the inner wall of the digestion tank is coated with a layer of polytetrafluoroethylene, and the digestion tank is made of a metal material.

In one or more embodiments, the mixed acid adding pipe is provided with a mixed acid control valve, and the raw material adding pipe is provided with a raw material control valve.

In one or more embodiments, a nitrogen control valve is provided on the nitrogen connection pipe, and a vacuum control valve is provided on the vacuum connection pipe.

In one or more embodiments, the acid liquor discharge pipe is provided with an acid liquor control valve, and the liquid outlet end of the acid liquor discharge pipe is provided with a liquid receiving vessel.

In one or more embodiments, the upper wall of the digestion tank is also provided with a pressure gauge and a pressure gauge control valve for controlling the pressure gauge switch.

In one or more embodiments, an electronic scale for weighing the change in weight of the digestion tank is provided on the heating device.

In one or more embodiments, the mixed acid adding pipe and the raw material adding pipe are provided with a first funnel and a second funnel at the adding ends, respectively.

Compared with the prior art, the closed digestion device for extracting metal ions of ethyl orthosilicate has the following advantages:

through having set up mixed acid on the digestion tank and added pipe and raw materials and added the pipe, avoided cross contamination, the device is small and exquisite be convenient for operate simultaneously, through setting up the vacuum connecting pipe, adopts vacuum system decompression to remove TEOS (tetraethoxysilane) and Si compound steam, reduces because the conflagration hidden danger and the operation risk that the intensification brought to accelerate TEOS and Si compound's discharge, can promote detection efficiency simultaneously, guarantee test repeatability. Through the nitrogen connecting pipe and the vacuum connecting pipe, the digestion tank can be well subjected to air impurity removal treatment

By reducing the redundant tank structure, the extraction mode of trace metal ions is optimized.

Drawings

FIG. 1 is a schematic view showing the structure of a sealed digestion device for extracting metal ions from ethyl orthosilicate according to an embodiment of the utility model.

The main reference numerals illustrate:

1. a first funnel; 2. a mixed acid adding pipe; 3. a mixed acid control valve; 4. a digestion tank; 5. a heating device; 6. an acid liquor discharge pipe; 7. an acid liquor control valve; 8. a liquid receiving vessel; 9. a vacuum connection tube; 10. a vacuum control valve; 11. a nitrogen control valve; 12. a nitrogen connecting pipe; 13. a raw material adding pipe; 14. a raw material control valve; 15. a pressure gauge control valve; 16. a pressure gauge; 17. and a second funnel.

Detailed Description

The following detailed description of embodiments of the utility model is, therefore, to be taken in conjunction with the accompanying drawings, and it is to be understood that the scope of the utility model is not limited to the specific embodiments.

Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.

As described in the background art, the existing system has a complex structure, more pipelines and more tank bodies, the requirements of ultra-clean rooms cannot be met, and the tank bodies are heated with the possibility of fire and high-temperature danger, so that the personal safety and the working efficiency of experimental operators can be seriously affected. According to the utility model, the mixed acid adding pipe, the raw material adding pipe, the nitrogen connecting pipe and the vacuum connecting pipe are arranged on the digestion tank, so that cross contamination is avoided, the whole device is simple in structure and convenient to operate, and the vacuum system is used for reducing pressure to remove TEOS (tetraethyl orthosilicate) and Si compound steam, so that fire hazards and operation risks caused by temperature rise are reduced, the detection efficiency is improved, and the test repeatability is ensured.

As shown in fig. 1, a sealed digestion device for extracting metal ions of ethyl orthosilicate according to an embodiment of the utility model includes a digestion tank 4. The upper wall of the digestion tank 4 is provided with a mixed acid adding pipe 2 and a raw material adding pipe 13 which are respectively used for adding mixed acid (acid mixture is abbreviated as mixed acid hereinafter) and raw materials into the digestion tank 4, and the arrangement mode is to independently add the mixed acid and the raw materials into the digestion tank 4 respectively so as to avoid cross contamination caused by different samples in the sampling process. The mixed acid adding pipe 2 is provided with a mixed acid control valve 3, and the raw material adding pipe 13 is provided with a raw material control valve 14. In addition, the digestion tank 4 is arranged on a heating device 5, and the heating device 5 is used for heating the mixed solution of the ethyl orthosilicate and the mixed acid in the digestion tank 4 so as to accelerate digestion of the ethyl orthosilicate.

In one embodiment, the inner wall of digestion tank 4 is coated with a layer of polytetrafluoroethylene that has good acid corrosion resistance. The digestion tank 4 is made of metal materials, so that the tank body of the digestion tank 4 has certain strength.

In an embodiment, a nitrogen connecting pipe 12 and a vacuum connecting pipe 9 are arranged on the side wall of the digestion tank 4, the nitrogen connecting pipe 12 is used for introducing nitrogen into the digestion tank 4, the vacuum connecting pipe 9 is used for pumping out the nitrogen and other miscellaneous gases in the digestion tank 4 until the digestion tank 4 is negative pressure, and the vacuum connecting pipe 9 is also used for pumping out the digested ethyl orthosilicate. In addition, a nitrogen control valve 11 is arranged on the nitrogen connecting pipe 12 and used for controlling the on-off of nitrogen, and a vacuum control valve 10 is arranged on the vacuum connecting pipe 9 and used for controlling the on-off of gas on the vacuum connecting pipe 9.

In one embodiment, the bottom wall of the digestion tank 4 is provided with an acid liquid discharge pipe 6, and the acid liquid discharge pipe 6 is used for discharging the mixed solution mixed with the metal to a specified position. An acid liquor control valve 7 is arranged on the acid liquor discharge pipe 6, and a liquid receiving vessel 8 is arranged at the liquid outlet end of the acid liquor discharge pipe 6. The upper wall of the digestion tank 4 is also provided with a pressure gauge 16 and a pressure gauge control valve 15 for controlling the opening and closing of the pressure gauge 16.

In order to facilitate recording of the weight change of the material in the digestion tank 4, an electronic scale for weighing the weight change of the digestion tank 4 is provided on the heating means 5.

In order to facilitate the addition of mixed acid and ethyl orthosilicate to the digestion tank 4, a first funnel 1 and a second funnel 17 are installed at the addition ends of the mixed acid addition pipe 2 and the raw material addition pipe 13, respectively.

through having set up mixed acid on digestion tank 4 and added pipe 2 and raw materials and added pipe 13, avoided cross contamination, the device is small and exquisite be convenient for operate simultaneously, through setting up vacuum connecting pipe 9, adopts vacuum system decompression to remove TEOS (tetraethoxysilane) and Si compound steam, has reduced fire hazard and operation risk because the intensification brings to accelerated TEOS and Si compound's discharge, can promote detection efficiency simultaneously, guarantee test repeatability. The digestion tank 4 can be well subjected to air impurity removal treatment through the nitrogen connecting pipe 12 and the vacuum connecting pipe 9.

The extraction mode of trace metal ions in the ethyl orthosilicate is optimized by reducing the redundant and redundant tank structure.

The working process of the closed digestion device for extracting metal ions of ethyl orthosilicate comprises the following steps:

firstly, all valves are closed, then the nitrogen control valve 11 and the pressure gauge control valve 15 are opened, nitrogen is introduced into the digestion tank 4 through the nitrogen connecting pipe 12, the pressure gauge 16 is observed until positive pressure is displayed, then the nitrogen control valve 11 is closed, the vacuum control valve 10 is opened to vacuumize the digestion tank 4 until the pressure gauge 16 is displayed as negative pressure, then the nitrogen control valve 11 is opened, nitrogen is introduced into the digestion tank 4, the steps are repeated for 3 times, so that the miscellaneous gas in the digestion tank 4 is removed, and finally, the nitrogen is introduced into the digestion tank 4 to make the pressure positive.

Then the nitrogen control valve 11 is closed, the mixed acid control valve 3 and the raw material control valve 14 are opened, mixed acid and ethyl orthosilicate are respectively added into the digestion tank 4 through the first funnel 1 and the second funnel 17, generally, the ethyl orthosilicate is added first, the weight is recorded through an electronic scale, then the mixed acid is added, and the weight is recorded. Then the mixed acid control valve 3 and the raw material control valve 14 are closed, the vacuum control valve 10 is opened to connect the digestion tank 4 into a vacuum system, and then the heating device 5 is started to heat the digestion tank 4, so that after all liquid substances are completely extracted from the system (generally, the weight of the electronic scale is observed to show no change and lasts for five minutes, the liquid substances in the digestion tank 4 are considered to be completely extracted). Then, the vacuum control valve 10 is closed, and the nitrogen control valve 11 is opened again to allow the digestion tank 4 to recover the positive pressure.

And finally, opening an acid mixing control valve 3, adding quantitative extracting solution through an acid mixing adding pipe 2, recording the weight by an electronic scale, opening an acid liquor control valve 7, and discharging the solution mixed with metal ions into a liquid receiving vessel 8 through an acid liquor discharging pipe 6 to finish the extraction of trace metal ions in the ethyl orthosilicate.

The foregoing descriptions of specific exemplary embodiments of the present utility model are presented for purposes of illustration and description. It is not intended to limit the utility model to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the utility model and its practical application to thereby enable one skilled in the art to make and utilize the utility model in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the utility model be defined by the claims and their equivalents.

Claims

1. A closed digestion device for extracting metal ions of tetraethoxysilane is characterized by comprising:

the digestion tank (4) is arranged on the heating device (5), the upper wall of the digestion tank (4) is provided with a mixed acid adding pipe (2) and a raw material adding pipe (13), the side wall of the digestion tank (4) is provided with a nitrogen connecting pipe (12) and a vacuum connecting pipe (9), and the bottom wall of the digestion tank (4) is provided with an acid liquor discharging pipe (6).

2. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein an inner wall of the digestion tank (4) is coated with a layer of polytetrafluoroethylene, and the digestion tank (4) is made of a metal material.

3. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein a mixed acid control valve (3) is provided on the mixed acid adding pipe (2), and a raw material control valve (14) is provided on the raw material adding pipe (13).

4. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein a nitrogen gas control valve (11) is provided on the nitrogen gas connection pipe (12), and a vacuum control valve (10) is provided on the vacuum connection pipe (9).

5. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein an acid liquor control valve (7) is provided on the acid liquor discharge pipe (6), and a liquid receiving vessel (8) is provided at a liquid outlet end of the acid liquor discharge pipe (6).

6. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein the upper wall of the digestion tank (4) is further provided with a pressure gauge (16) and a pressure gauge control valve (15) for controlling the opening and closing of the pressure gauge (16).

7. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein an electronic scale for weighing the weight change of the digestion tank (4) is provided on the heating device (5).

8. The sealed digestion device for extracting metal ions of ethyl orthosilicate as set forth in claim 1, wherein the addition ends of the mixed acid addition pipe (2) and the raw material addition pipe (13) are respectively provided with a first funnel (1) and a second funnel (17).