CN112279271A - Device and process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia - Google Patents

Device and process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia Download PDF

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Publication number
CN112279271A
CN112279271A CN202011276154.5A CN202011276154A CN112279271A CN 112279271 A CN112279271 A CN 112279271A CN 202011276154 A CN202011276154 A CN 202011276154A CN 112279271 A CN112279271 A CN 112279271A
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China
Prior art keywords
ammonia
communicated
tower
absorption tower
purge gas
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CN202011276154.5A
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Chinese (zh)
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甘世杰
王恩伟
张昌艳
李冬
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Henan Junhua Development Co ltd
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Henan Junhua Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/024Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/022Preparation of aqueous ammonia solutions, i.e. ammonia water
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/10Separation of ammonia from ammonia liquors, e.g. gas liquors

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a device and a process for producing electronic-grade ammonia water by utilizing synthetic ammonia purge gas. The process comprises the following steps: (1) the synthetic ammonia purge gas enters a pre-absorption tower, and flows upwards in a counter-current manner to pass through the pre-absorption tower for washing to obtain a crude ammonia water solution; (2) the crude ammonia water solution in the step (1) enters a heat exchanger to be heated, then enters an ammonia still to carry out ammonia-water separation, and tower top liquid obtained by the ammonia still enters an absorption tower and a washing tower to be treated and then enters an absorption tower; (3) and (3) filtering the ammonia water solution in the absorption tower in the step (2) through a membrane to obtain electronic-grade ammonia water. The device provided by the invention has a simple structure, fully utilizes the purge gas of the synthetic ammonia, has a reasonable design, reduces the waste of the purge gas, and can produce electronic-grade ammonia water.

Description

Device and process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia
Technical Field
The invention belongs to the technical field of ammonia water preparation, and particularly relates to a device and a process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia.
Background
In the synthetic ammonia production process, hydrogen and nitrogen are used as raw materials for synthesizing ammonia. The nitrogen separated from the air reacts with hydrogen obtained by conversion or gasification of natural gas at elevated pressure and temperature and with the action of a catalyst to produce ammonia. Generally, due to the limitation of chemical equilibrium, reactants cannot be completely converted, and unreacted nitrogen and hydrogen are mixed with supplemented fresh gas through a recycle compressor and then enter a synthesis tower as recycle gas to participate in the synthesis ammonia reaction again. Since the raw material gas for synthesis ammonia contains a certain amount of inert components of argon and methane, which are accumulated continuously in the circulation process, not only the circulation compression work is consumed, but also the effective volume of the synthesis tower is reduced, and the normal reaction of the synthesis ammonia is influenced, a part of the mixed gas of the synthesis tower must be discharged to control the concentration of the inert components of argon and methane in the synthesis tower, and the part of the discharged gas is called as the purge gas of the synthesis ammonia. The amount of discharged gas is about 300N square meters per ton of ammonia, and the typical composition of the gas is: 50-70% H2(V/V),1~8%NH3(V/V),18~25%N2(V/V), the remainder being methane and argon. The purge gas of the existing domestic ammonia synthesis device is directly sent out of the ammonia synthesis system after being decompressed, and the purge gas contains a large amount of unreacted hydrogen and nitrogen, so that the effective components in the purge gas are not fully utilized, and a lot of resource waste is caused.
The electronic-grade ammonia water is an alkaline cleaning and corrosive agent, can be prepared and used with hydrogen peroxide, water and hydrofluoric acid, and is mainly used for the production of a super-large-scale integrated circuit process technology.
Therefore, in order to solve the above problems, it is possible to design an apparatus capable of producing electronic-grade ammonia water using the purge gas of synthesis ammonia.
Disclosure of Invention
The invention aims to provide a device for producing electronic-grade ammonia water by utilizing purge gas of synthetic ammonia, which has the advantages of simple structure, reasonable design, convenient use, safety and high efficiency, and provides a production process thereof, and the device has the advantages of simple process, flexible operation and high production efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that:
a device for producing electronic-grade ammonia water by utilizing synthetic ammonia purge gas comprises a purge gas pre-absorption system, wherein the purge gas pre-absorption system is communicated with an ultrapure water washing absorption system, the ultrapure water washing absorption system is communicated with a membrane filtration system, and the membrane filtration system is communicated with an electronic-grade ammonia water storage tank;
the purge gas pre-absorption system comprises a pre-absorption tower, a material outlet of the pre-absorption tower is communicated with a first material inlet of a heat exchanger, a first material outlet of the heat exchanger is communicated with a first material inlet of an ammonia still, and a first material outlet of the ammonia still is communicated with a material inlet of an adsorption tower;
the ultrapure water washing absorption system comprises a washing tower, wherein a material inlet of the washing tower is communicated with a material outlet of the adsorption tower, a material outlet of the washing tower is communicated with a first material inlet of the absorption tower, a material outlet of the absorption tower is communicated with a material inlet of the membrane filtration system, and a material outlet of the membrane filtration system is communicated with a material inlet of the electronic-grade ammonia water storage tank.
And further, a second material outlet of the ammonia still is communicated with a second material inlet of the heat exchanger through an ammonia still kettle pump, and the second material outlet of the heat exchanger is communicated with a second material inlet of the pre-absorption tower.
Further, a second material outlet of the ammonia still is communicated with a material inlet of the reboiler through the ammonia still kettle pump, and a material outlet of the reboiler is communicated with a second material inlet of the ammonia still.
Furthermore, a material outlet of the absorption tower is communicated with a material inlet of a condenser through a tower kettle pump, and a material outlet of the condenser is communicated with a second material inlet of the absorption tower.
Furthermore, an ultrapure water inlet of the washing tower is communicated with an ultrapure water device, and the ultrapure water device is also communicated with an ultrapure water inlet of the absorption tower.
Furthermore, a fuel gas outlet of the pre-absorption tower is communicated with a fuel gas recovery device, and the fuel gas recovery device is also communicated with a fuel gas outlet of the absorption tower.
Further, an ammonia water outlet of the washing tower is communicated with a reagent-grade ammonia water storage tank.
A process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia comprises the following steps:
(1) the synthetic ammonia purge gas enters a pre-absorption tower, and flows upwards in a counter-current manner to pass through the pre-absorption tower for washing to obtain a crude ammonia water solution;
(2) the crude ammonia water solution in the step (1) enters a heat exchanger to be heated, then enters an ammonia still to carry out ammonia-water separation, and tower top liquid obtained by the ammonia still enters an absorption tower and a washing tower to be treated and then enters an absorption tower;
(3) and (3) filtering the ammonia water solution in the absorption tower in the step (2) through a membrane to obtain electronic-grade ammonia water.
Further, the tower bottom solution of the ammonia still in the step (2) enters the upper part of the pre-absorption tower through a heat exchanger.
Further, the temperature of the crude ammonia water solution in the step (2) in the heat exchanger is 140-200 ℃.
The invention has the advantages that:
the device and the process for producing the electronic-grade ammonia water by using the purge gas of the synthetic ammonia have the advantages of simple structure, reasonable design, reduction of waste of the purge gas and capability of producing the electronic-grade ammonia water, and the purge gas of the synthetic ammonia is fully utilized.
The synthetic ammonia purge gas enters from the bottom of the pre-absorption tower, flows upwards in a counter-current manner, is washed by water in the pre-absorption tower to remove ammonia gas, and then is sent to a fuel gas recovery device. And (3) the ammonia water solution obtained at the tower bottom of the pre-absorption tower is subjected to heat exchange by a heat exchanger and heated to 140-200 ℃, enters an ammonia still for treatment, the concentration of the ammonia water solution obtained at the tower bottom of the pre-absorption tower is 5-25wt%, and enters the ammonia still for ammonia-water separation. The component with ammonia content of about 99.5wt% is obtained at the top of the ammonia still, the component with ammonia concentration lower than 100ppm is obtained at the bottom of the ammonia still, and the component is pumped into the heat exchanger and the pre-heater from the bottom of the ammonia stillAnd the kettle liquid of the absorption tower enters the pre-absorption tower for cyclic utilization after heat exchange. The reboiler provides heat source for the ammonia still, and the components with ammonia content of 99.5wt% obtained from the top of the ammonia still are treated in the adsorption tower to eliminate partial impurity and water and obtain pure ammonia gas. Then enters a washing tower from the bottom of the washing tower, is fully washed by ultrapure water to remove impurities such as metal ions in the ammonia gas, and then is sent into an absorption tower, and reagent-grade ammonia water (NH in the reagent-grade ammonia water) is generated at the lower part of the absorption tower3Content 25-28%) flows into a reagent-grade ammonia water storage tank. The top of the absorption tower is also used for fully absorbing the ammonia gas by the reverse contact of ultrapure water and the ammonia gas, then the ammonia water with higher purity is obtained, the absorption tower is connected with a condenser to absorb heat, the temperature of the whole circulating system is reduced to control the temperature constancy of the whole circulating system, and the temperature rise of the system is prevented from being too high. And finally, further purifying by a membrane filtration system to obtain electronic-grade ammonia water, wherein the electronic-grade ammonia water contains metal ions with the concentration of about 1-10 ppt.
Drawings
FIG. 1 is a schematic diagram of the system of the present invention.
Detailed Description
As shown in figure 1, the invention discloses a device for producing electronic-grade ammonia water by using synthetic ammonia purge gas, which comprises a purge gas pre-absorption system A, wherein the purge gas pre-absorption system A is communicated with an ultrapure water washing absorption system B, the ultrapure water washing absorption system B is communicated with a membrane filtration system 14, and the membrane filtration system 14 is communicated with an electronic-grade ammonia water storage tank 15.
The purge gas pre-absorption system comprises a pre-absorption tower 1, and a fuel gas outlet 101 of the pre-absorption tower is communicated with a fuel gas recovery device 2. The material outlet 102 of the pre-absorption tower is communicated with a first material inlet 301 of a heat exchanger, the first material outlet 302 of the heat exchanger is communicated with a first material inlet 401 of an ammonia still, and the first material outlet 402 of the ammonia still is communicated with a material inlet 501 of an adsorption tower. The second material outlet 403 of the ammonia still is communicated with the second material inlet 303 of the heat exchanger through the ammonia still pump 6, and the second material outlet 304 of the heat exchanger is communicated with the second material inlet 103 of the pre-absorption tower. The second material outlet 403 of the ammonia still is communicated with a reboiler material inlet 701 through an ammonia still kettle pump 6, and the reboiler material outlet 702 is communicated with the second material inlet 404 of the ammonia still.
The ultrapure water washing absorption system comprises a washing tower 8, wherein a material outlet 502 of the adsorption tower is communicated with a material inlet 801 of the washing tower, an ultrapure water inlet 802 of the washing tower is communicated with an ultrapure water device 9, and an ammonia water outlet 803 of the washing tower is communicated with a reagent-grade ammonia water storage tank 10. The material outlet 804 of the washing tower is communicated with a first material inlet 1101 of the absorption tower, the material outlet 1102 of the absorption tower is communicated with a condenser material inlet 1301 through a tower kettle pump 12, the material outlet 1302 of the condenser is communicated with a second material inlet 1103 of the absorption tower, the ultrapure water inlet 1104 of the absorption tower is communicated with an ultrapure water device 9, and the fuel gas outlet 1105 of the absorption tower is communicated with a fuel gas recovery device 2. The material outlet 1102 of the absorption tower is communicated with a material inlet 1401 of the membrane filtration system, and the material outlet 1402 of the membrane filtration system is communicated with a material inlet of the electronic-grade ammonia water storage tank 15.
A process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia comprises the following steps:
(1) the synthetic ammonia purge gas enters the pre-absorption tower 1 from a first material inlet 104 of the pre-absorption tower, and flows upwards in a counter-current manner to pass through the pre-absorption tower 1 for water washing, so that crude ammonia water solution is obtained.
(2) The crude ammonia water solution in the step (1) enters a heat exchanger 3 to be heated to 140 ℃ and 200 ℃, then enters an ammonia still 4 to carry out ammonia-water separation, a reboiler 7 provides a heat source for the ammonia still 4, a tower kettle solution of the ammonia still 4 enters the upper part of a pre-absorption tower 1 through the heat exchanger 3, a tower top liquid obtained from the ammonia still 4 enters an absorption tower 5 and a washing tower 8 to be treated, and then enters an absorption tower 11, and the absorption tower 11 is connected with a condenser 13 to absorb heat.
(3) And (3) filtering the ammonia water solution in the absorption tower 11 in the step (2) through a membrane to obtain electronic-grade ammonia water.

Claims (10)

1. The utility model provides an utilize synthetic ammonia to purge device of gassing production electronic grade aqueous ammonia which characterized in that: the device comprises a purge gas pre-absorption system, wherein the purge gas pre-absorption system is communicated with an ultrapure water washing absorption system, the ultrapure water washing absorption system is communicated with a membrane filtration system, and the membrane filtration system is communicated with an electronic-grade ammonia water storage tank;
the purge gas pre-absorption system comprises a pre-absorption tower, a material outlet of the pre-absorption tower is communicated with a first material inlet of a heat exchanger, a first material outlet of the heat exchanger is communicated with a first material inlet of an ammonia still, and a first material outlet of the ammonia still is communicated with a material inlet of an adsorption tower;
the ultrapure water washing absorption system comprises a washing tower, wherein a material inlet of the washing tower is communicated with a material outlet of the adsorption tower, a material outlet of the washing tower is communicated with a first material inlet of the absorption tower, a material outlet of the absorption tower is communicated with a material inlet of the membrane filtration system, and a material outlet of the membrane filtration system is communicated with a material inlet of the electronic-grade ammonia water storage tank.
2. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and a second material outlet of the ammonia still is communicated with a second material inlet of the heat exchanger through an ammonia still kettle pump, and a second material outlet of the heat exchanger is communicated with a second material inlet of the pre-absorption tower.
3. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and a second material outlet of the ammonia still is communicated with a material inlet of the reboiler through an ammonia still kettle pump, and a material outlet of the reboiler is communicated with a second material inlet of the ammonia still.
4. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and the material outlet of the absorption tower is communicated with the material inlet of the condenser through a tower kettle pump, and the material outlet of the condenser is communicated with the second material inlet of the absorption tower.
5. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and the ultrapure water inlet of the washing tower is communicated with an ultrapure water device, and the ultrapure water device is also communicated with the ultrapure water inlet of the absorption tower.
6. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and the fuel gas outlet of the pre-absorption tower is communicated with a fuel gas recovery device, and the fuel gas recovery device is also communicated with the fuel gas outlet of the absorption tower.
7. The apparatus for producing electronic grade ammonia water using synthesis ammonia purge gas according to claim 1, wherein: and an ammonia water outlet of the washing tower is communicated with a reagent-grade ammonia water storage tank.
8. A process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia is characterized by comprising the following steps: the method comprises the following steps:
(1) the synthetic ammonia purge gas enters a pre-absorption tower, and flows upwards in a counter-current manner to pass through the pre-absorption tower for washing to obtain a crude ammonia water solution;
(2) the crude ammonia water solution in the step (1) enters a heat exchanger to be heated, then enters an ammonia still to carry out ammonia-water separation, and tower top liquid obtained by the ammonia still enters an absorption tower and a washing tower to be treated and then enters an absorption tower;
(3) and (3) filtering the ammonia water solution in the absorption tower in the step (2) through a membrane to obtain electronic-grade ammonia water.
9. The process for producing electronic grade ammonia water by using synthesis ammonia purge gas as claimed in claim 8, wherein: and (3) the tower kettle solution of the ammonia still in the step (2) enters the upper part of the pre-absorption tower through the heat exchanger.
10. The process for producing electronic grade ammonia water using synthesis ammonia purge gas as claimed in claim 8, wherein: the temperature rise temperature of the crude ammonia water solution in the step (2) in the heat exchanger is 140-200 ℃.
CN202011276154.5A 2020-11-16 2020-11-16 Device and process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia Pending CN112279271A (en)

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CN202011276154.5A CN112279271A (en) 2020-11-16 2020-11-16 Device and process for producing electronic-grade ammonia water by using purge gas of synthetic ammonia

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114644348A (en) * 2022-03-18 2022-06-21 西安吉利电子新材料股份有限公司 Preparation system and method for directly producing electronic-grade ammonia water from ammonia gas

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203728571U (en) * 2013-12-18 2014-07-23 大连欧科膜技术工程有限公司 Device for recovering hydrogen and ammonia in purge gas of synthesis ammonia
CN105523570A (en) * 2016-02-16 2016-04-27 江苏达诺尔科技股份有限公司 Preparation method of ppt-scale ultrapure ammonium hydroxide
CN109319736A (en) * 2018-10-09 2019-02-12 四川金象赛瑞化工股份有限公司 Ammonia tank periodic off-gases recyclable device and its technique
CN109850917A (en) * 2018-12-26 2019-06-07 江苏达诺尔科技股份有限公司 A kind of preparation method of efficient low-consume PPT grades of high-purity ammonia waters

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203728571U (en) * 2013-12-18 2014-07-23 大连欧科膜技术工程有限公司 Device for recovering hydrogen and ammonia in purge gas of synthesis ammonia
CN105523570A (en) * 2016-02-16 2016-04-27 江苏达诺尔科技股份有限公司 Preparation method of ppt-scale ultrapure ammonium hydroxide
CN109319736A (en) * 2018-10-09 2019-02-12 四川金象赛瑞化工股份有限公司 Ammonia tank periodic off-gases recyclable device and its technique
CN109850917A (en) * 2018-12-26 2019-06-07 江苏达诺尔科技股份有限公司 A kind of preparation method of efficient low-consume PPT grades of high-purity ammonia waters

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114644348A (en) * 2022-03-18 2022-06-21 西安吉利电子新材料股份有限公司 Preparation system and method for directly producing electronic-grade ammonia water from ammonia gas
CN114644348B (en) * 2022-03-18 2023-12-12 西安吉利电子新材料股份有限公司 Preparation system and method for directly producing electronic grade ammonia water from ammonia gas

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