CN216946235U - Preparation system for directly producing electronic-grade ammonia water from ammonia gas - Google Patents
Preparation system for directly producing electronic-grade ammonia water from ammonia gas Download PDFInfo
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- CN216946235U CN216946235U CN202220601282.0U CN202220601282U CN216946235U CN 216946235 U CN216946235 U CN 216946235U CN 202220601282 U CN202220601282 U CN 202220601282U CN 216946235 U CN216946235 U CN 216946235U
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The utility model belongs to the technical field of electronic chemistry, and particularly discloses a preparation system for directly producing electronic-grade ammonia water from ammonia gas, which comprises a raw material storage tank, a cleaning tower, a distillation tower, an absorption tower and a microporous filter membrane which are sequentially communicated through a pipeline; a pressurizing device is arranged between the cleaning tower and the distillation tower; the pressurizing equipment is connected with the cleaning tower and the distillation tower through pipelines; the interior of the cleaning tower and the interior of the absorption tower are both high-purity water; the absorption tower is used for carrying out the reaction of ammonia gas and high-purity water. The high-purity ammonia with extremely high purity can be obtained by utilizing the ammonia purification process of the utility model, so that the electronic-grade ammonia water is prepared, and the impurities in the ammonia water are reduced.
Description
Technical Field
The utility model belongs to the technical field of electronic chemistry, and particularly relates to a preparation system for directly producing electronic-grade ammonia water from ammonia gas.
Background
In recent years, rapid development of the electronic industry drives rapid development of electronic-grade ammonia water production, and the development of the electronic-grade ammonia water industry enters a new stage. The electronic-grade ammonia water is mainly used for cleaning in the electronic industry and synthesizing downstream compounds of the electronic-grade ammonia water. With the rapid development of high-end semiconductor materials, LED materials and solar materials in China, the demand of electronic-grade ammonia water is greatly increased.
The electronic-grade ammonia water is prepared by introducing high-purity ammonia into high-purity water for absorption and then treating the ammonia water by a microporous filter membrane. The key element of the synthesis of the electronic-grade ammonia water is the preparation of high-purity ammonia. At present, high-purity ammonia produced by a large-scale process is mostly adopted as a raw material in the market. The method has the advantages of high price, large investment specific gravity of raw materials and high cost. The industrial ammonia gas has low price, but the ammonia water prepared by directly using the industrial ammonia gas has more impurities and can not reach the electronic grade.
Therefore, it is an urgent technical problem to be solved by those skilled in the art to provide a new electronic grade ammonia water preparation system.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defect of difficulty in preparation of electronic-grade ammonia water in the prior art, and provides a preparation system for directly producing electronic-grade ammonia water from ammonia gas.
The utility model provides a preparation system for directly producing electronic-grade ammonia water from ammonia gas, which comprises a raw material storage tank, a cleaning tower, a distillation tower, an absorption tower and a microporous filter membrane which are sequentially communicated through a pipeline, wherein the raw material storage tank is used for containing industrial ammonia gas;
a pressurizing device is arranged between the cleaning tower and the distillation tower;
the pressurizing equipment is respectively connected with the cleaning tower and the distillation tower through pipelines;
the cleaning medium/absorbing medium of the cleaning tower and the absorbing tower is high-purity water;
the absorption tower is used for carrying out the reaction of ammonia gas and high-purity water.
According to a further scheme, the system further comprises a collecting device;
the collecting device is communicated with the cleaning tower and the distillation tower through collecting pipelines respectively and is used for collecting the cleaning reflux liquid of the cleaning tower and the liquid at the bottom of the distillation tower.
The further proposal is that the collecting pipeline is provided with a one-way valve.
The further scheme is that the cleaning tower comprises a first cleaning tower and a second cleaning tower;
the first cleaning tower and the second cleaning tower are communicated through a pipeline, the air inlet end of the first cleaning tower is communicated with the raw material storage tank, and the air outlet end of the second cleaning tower is communicated with the pressurizing equipment.
In a further scheme, a molecular sieve and a resin column are arranged between the distillation tower and the absorption tower;
the molecular sieve is communicated with the resin column through a pipeline, the gas inlet end of the molecular sieve is communicated with the distillation tower, and the gas outlet end of the resin column is communicated with the absorption tower.
In a further scheme, cooling equipment is also arranged between the absorption tower and the microporous filter membrane;
the cooling equipment is communicated with the absorption tower and the microporous filter membrane through a pipeline.
In a further scheme, the molecular sieve is a 3A molecular sieve, and the resin column is lithium-based resin.
The further scheme is that a cleaning tower, a distillation tower, an absorption tower, a product storage tank, a collecting device, pressurizing equipment, a molecular sieve shell, a resin column, cooling equipment, a one-way valve, microporous filter membrane treatment equipment and a connecting pipeline which are involved in the purification and preparation processes all adopt polytetrafluoroethylene as linings, gaskets at flange joints and all devices contacted by raw materials in the whole preparation process all adopt polytetrafluoroethylene materials, and other impurities cannot be brought in the whole process.
Compared with the prior art, the utility model has the beneficial effects that:
(1) the utility model is used as a special preparation system of electronic-grade ammonia water, combines a raw material purification system with an ammonia water production system, and starts to purify raw materials when in use, thereby reducing the production cost of the electronic-grade ammonia water.
(2) The method can obtain high-purity ammonia gas with extremely high purity through cleaning of a two-stage cleaning tower, distillation of a distillation tower, adsorption of a molecular sieve and a resin column, so that electronic-grade ammonia water is prepared, and impurities in the ammonia water are reduced.
(3) The method for preparing the electronic-grade ammonia water is easy to realize, reduces the preparation cost of the electronic-grade ammonia water, can realize industrial production, and can continuously prepare the electronic-grade ammonia water.
Drawings
The utility model is illustrated and described only by way of example and not by way of limitation in the scope of the utility model as set forth in the following drawings, in which:
FIG. 1: the preparation system of the utility model is connected with the structure schematic diagram;
in the figure: 1 a first cleaning tower, 2 a second cleaning tower, 3a distillation tower, 4 an absorption tower, 5 a microporous filter membrane, 6 a product storage tank, 7 a collecting device, 8 a pressurizing device, 9 a molecular sieve, 10 a resin column and 11 a cooling device.
Detailed Description
In order to make the objects, technical solutions, design methods, and advantages of the present invention more apparent, the present invention will be further described in detail by specific embodiments with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and are not intended to limit the utility model.
Example 1
As shown in fig. 1, the utility model provides a preparation system for directly producing electronic-grade ammonia water from ammonia gas, which comprises a raw material storage tank, a cleaning tower, a distillation tower 3, an absorption tower 4 and a microporous filter membrane 5 which are sequentially communicated through a pipeline, wherein the raw material storage tank is used for containing industrial ammonia gas;
a pressurizing device 8 is arranged between the cleaning tower and the distillation tower 3;
the pressurizing device 8 is connected with the cleaning tower and the distillation tower 3 through pipelines;
the inside of the cleaning tower and the inside of the absorption tower 4 are both high-purity water;
the absorption tower 4 is used for carrying out the reaction of ammonia gas and high-purity water.
Optionally, the system further comprises a collecting device 7;
the collecting device 7 is communicated with the cleaning tower and the distillation tower 3 through collecting pipelines respectively and is used for collecting the cleaning reflux liquid of the cleaning tower and the bottom liquid of the distillation tower 3.
The collecting pipe is provided with a one-way valve 12 for placing the collected liquid to flow backwards, and it should be understood that a water pump should be arranged inside the collecting device 7 for accelerating the collection of the recovered liquid.
In the present embodiment, the purge tower includes a first purge tower 1 and a second purge tower 2;
the first cleaning tower 1 and the second cleaning tower 2 are communicated through a pipeline, the air inlet end of the first cleaning tower 1 is communicated with the raw material storage tank, the air outlet end of the second cleaning tower 2 is communicated with the pressurizing device 8, one third of high-purity water with the volume of the cleaning towers is introduced into the two cleaning towers, the resistivity of the high-purity water is more than or equal to 18M omega cm, and it should be understood that the air inlet pipeline of the first cleaning tower 1 is arranged below the level of the high-purity water, and the air inlet pipeline of the second cleaning tower 2 is arranged below the level of the high-purity water.
Optionally, a molecular sieve 9 and a resin column 10 are further arranged between the distillation tower 3 and the absorption tower 4; the molecular sieve 9 is communicated with the resin column 10 through a pipeline, the gas inlet end of the molecular sieve 9 is communicated with the distillation tower 3, and the gas outlet end of the resin column 10 is communicated with the absorption tower 4. A cooling device 11 is also arranged between the absorption tower 4 and the microporous filter membrane 5; the cooling device 11 is communicated with the absorption tower 4 and the microporous filter membrane 5 through a pipeline, and the microporous filter membrane 5 is communicated with the product storage tank 6 through a pipeline and used for collecting the filtered electronic-grade ammonia water.
Optionally, the molecular sieve 9 is a 3A molecular sieve, and the resin column 10 is a lithium-based resin.
The cleaning tower, the distillation tower, the absorption tower, the product storage tank, the collecting device, the pressurizing device, the molecular sieve shell, the resin column, the cooling device, the one-way valve, the microporous membrane treatment device and the connecting pipeline which are involved in the purification and preparation processes all adopt polytetrafluoroethylene as linings, and all devices which are contacted by raw materials in the whole preparation process and gaskets at the flange joint are made of polytetrafluoroethylene materials, so that other impurities cannot be brought in the whole preparation process.
When the utility model is used, at least the following steps are included:
step 1, introducing industrial ammonia gas into a cleaning tower, and when ultrapure water in the cleaning tower is absorbed to a saturated state, continuing introducing the industrial ammonia gas to obtain mixed gas I containing the ammonia gas;
and 4, filtering the mixture III by using a microporous filter membrane to obtain electronic-grade ammonia water.
Specifically, in the step 1, the ammonia gas with higher purity obtained by cleaning in the two-stage cleaning tower is converted into liquid ammonia by the pressurizing equipment, and in the step 2, the liquid ammonia is input into the distillation tower, and grease, nitrogen, carbon dioxide, sulfide, a small amount of water and more metal examples in the ammonia gas are further removed by distillation, so that the ammonia gas with extremely high purity is obtained. Wherein the pressure of the pressurizing device for changing the gaseous ammonia into the liquid ammonia is 2.0MPa, the temperature in the distillation tower is 33.5 ℃, and the pressure is 1.5 MPa.
And 3, cleaning by a two-stage cleaning tower and distilling by a distillation tower to obtain the ammonia gas with extremely high purity, and further removing a few residual metal ions in the ammonia gas by molecular sieve adsorption and resin column adsorption to obtain the high-purity ammonia gas with extremely high purity. Wherein the molecular sieve is a 3A molecular sieve, the resin is lithium-based resin, the adsorption temperature is 30 ℃, and the pressure is 3.5 MPa.
And 4, cleaning by a two-stage cleaning tower, distilling by a distillation tower, adsorbing by a molecular sieve and a resin column to obtain high-purity ammonia gas with extremely high purity, introducing the obtained high-purity ammonia gas into an absorption tower filled with high-purity water for absorption, and preparing the semi-finished product of the electronic-grade ammonia water. Wherein the resistivity of the high-purity water is more than or equal to 18M omega cm, the gas-water ratio is 2:5, the pressure in the absorption tower is 0.4MPa, and the concentration of the prepared ammonia water is 29 percent.
In the steps, the semi-finished product of the electronic-grade ammonia water prepared by the absorption tower is cooled by cooling equipment, and then is treated by a microporous filter membrane to prepare the finished product of the electronic-grade ammonia water. Wherein the temperature is cooled to less than or equal to 25 ℃, ammonia gas in the ammonia water is prevented from volatilizing, the concentration of the ammonia water is increased, the aperture of the microporous filter membrane is 0.05 mu m, the pressure is 0.55MPa, and the material of the microporous filter membrane is polytetrafluoroethylene.
And (3) processing the electronic grade ammonia water finished product by using a microporous filter membrane to prepare the finished product, and sampling and detecting: wherein the content of all metal ions is less than or equal to 50PPt, the content of anions is less than or equal to 40PPb, and the number of particles (more than or equal to 0.5 μm) is less than or equal to 25/mL.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (7)
1. A preparation system for directly producing electronic-grade ammonia water from ammonia gas is characterized by comprising a raw material storage tank, a cleaning tower, a distillation tower (3), an absorption tower (4) and a microporous filter membrane (5) which are sequentially communicated through a pipeline;
a pressurizing device (8) is arranged between the cleaning tower and the distillation tower (3);
the pressurizing equipment (8) is respectively connected with the cleaning tower and the distillation tower (3) through pipelines;
the cleaning medium/absorbing medium of the cleaning tower and the absorbing tower (4) is high-purity water;
the absorption tower (4) is used for carrying out the reaction of ammonia gas and high-purity water.
2. A production system for the direct production of electronic grade ammonia water from ammonia gas according to claim 1, characterized in that it further comprises a collection device (7);
the collecting device (7) is communicated with the cleaning tower and the distillation tower (3) through collecting pipelines respectively and is used for collecting the cleaning reflux liquid of the cleaning tower and the bottom liquid of the distillation tower (3).
3. A system for the production of electronic grade ammonia water directly from ammonia gas according to claim 2, characterized in that the collection pipe is provided with a non-return valve (12).
4. A production system for the direct production of electronic grade ammonia water from ammonia gas according to claim 1, characterized in that said washing column comprises a first washing column (1) and a second washing column (2);
the first cleaning tower (1) is communicated with the second cleaning tower (2) through a pipeline, the air inlet of the first cleaning tower (1) is communicated with the raw material storage tank, and the air outlet of the second cleaning tower (2) is communicated with the pressurizing equipment (8).
5. The system for the preparation of electronic grade ammonia water directly from ammonia gas according to claim 1, characterized in that a molecular sieve (9) and a resin column (10) are arranged between the distillation column (3) and the absorption column (4) in sequence;
the molecular sieve (9) is communicated with the resin column (10) through a pipeline, the gas inlet end of the molecular sieve (9) is communicated with the distillation tower (3), and the gas outlet end of the resin column (10) is communicated with the absorption tower (4).
6. A system for preparing electronic grade ammonia water directly from ammonia gas according to claim 1, characterized in that a cooling device (11) is arranged between the absorption tower (4) and the microporous membrane (5);
the cooling device (11) is respectively communicated with the absorption tower (4) and the microporous filter membrane (5) through pipelines.
7. A production system for directly producing electronic grade ammonia water from ammonia gas according to claim 5, characterized in that the molecular sieve (9) is 3A molecular sieve and the resin column (10) is lithium-based resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220601282.0U CN216946235U (en) | 2022-03-18 | 2022-03-18 | Preparation system for directly producing electronic-grade ammonia water from ammonia gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220601282.0U CN216946235U (en) | 2022-03-18 | 2022-03-18 | Preparation system for directly producing electronic-grade ammonia water from ammonia gas |
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| Publication Number | Publication Date |
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| CN216946235U true CN216946235U (en) | 2022-07-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202220601282.0U Active CN216946235U (en) | 2022-03-18 | 2022-03-18 | Preparation system for directly producing electronic-grade ammonia water from ammonia gas |
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| CN (1) | CN216946235U (en) |
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- 2022-03-18 CN CN202220601282.0U patent/CN216946235U/en active Active
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