Device for co-producing ultra-pure ammonia and electronic-grade ammonia water

Abstract

The utility model relates to a device for co-producing ultra-pure ammonia and electronic-grade ammonia water. Comprising a raw material storage tank, an ultra-pure ammonia product storage tank and an electronic grade ammonia water storage tank, the raw material storage tank is connected with the ultra-pure ammonia product storage tank through a rectification unit, the rectification unit comprises a light component removal rectification tower and a heavy component removal rectification tower, and a gas phase outlet of the heavy component removal rectification tower is connected with a first tube pass of a composite condenser through a first tee joint; a first tube pass of the composite condenser is connected with a liquid storage tank; the liquid storage tank is respectively connected with a reflux inlet of the de-heavy rectifying tower and an ultra-pure ammonia product storage tank; the third end of the first tee joint is connected with an electronic-grade ammonia water storage tank through an electronic-grade ammonia water preparation part; according to the utility model, the electronic-grade ammonia water is produced based on an ultra-pure ammonia production system, and the production can flexibly adjust the ultra-pure ammonia and the electronic-grade ammonia water so as to meet the fluctuation of market price, thereby achieving the characteristic of improving the economic benefits of enterprises.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of ultrapure ammonia production, in particular to a device for co-production of ultrapure ammonia and electronic grade ammonia water. BACKGROUND

[0002] At present, most of the domestic electronic grade ammonia water production processes use industrial ammonia as raw material for production. In the production process, heating evaporation vaporization and adsorption impurity removal processes are commonly used to achieve it. For details, see Chinese patent publication No. CN115504486A, which discloses a production method of ultrahigh-purity electronic grade ammonia water. Industrial liquid ammonia is subjected to two-stage filtration, oxidation, vaporization, purification, adsorption, filtration, hydration absorption, filtration and other processes. First, the liquid ammonia passes through the eccentric jet micro-porous reactor, and an oxidizing solution is added in the reactor to remove reducing substances in the ammonia water. The ammonia water with easy oxidation is filtered through a wire mesh filter and activated carbon, and then enters the vaporizer. The liquid ammonia is vaporized in the vaporizer. The vaporized ammonia gas enters the adsorption tower after passing through the purification chamber, and then enters the co-current absorption tower through the filter at the top of the adsorption tower. The ammonia water intermediate product is obtained by passing through the co-current absorption tower. The synthesized ammonia water is filtered through a microporous membrane to obtain G5 grade high-purity electronic grade ammonia water. The above process has the defects of complex process and high energy consumption. Further, with the change of market environment, the price of electronic grade ammonia water is prone to fluctuate. How to reduce production cost during the period when the price of electronic grade ammonia water is high has become a technical problem to be solved in the industry. SUMMARY

[0003] In order to make up for the above shortcomings, the utility model provides a device for co-production of ultrapure ammonia and electronic grade ammonia water to solve the technical problems existing in the prior art.

[0004] The technical scheme adopted by the utility model to solve its technical problems is:

[0005] A device for co-production of ultrapure ammonia and electronic grade ammonia water, the device comprises a raw material storage tank, an ultrapure ammonia product storage tank and an electronic grade ammonia water storage tank, the raw material storage tank is connected with the ultrapure ammonia product storage tank through a rectification unit, the rectification unit comprises a light-removing rectification tower and a heavy-removing rectification tower, the gas phase outlet of the heavy-removing rectification tower is connected with the first tube pass of a composite condenser through a first three-way joint, the first tube pass of the composite condenser is connected with a liquid storage tank, and the liquid storage tank is connected with the reflux liquid inlet of the heavy-removing rectification tower and the ultrapure ammonia product storage tank respectively; the third end of the first three-way joint is connected with the electronic grade ammonia water preparation part and the electronic grade ammonia water storage tank.

[0006] The utility model discloses an electronic grade ammonia water production system based on ultrapure ammonia production system, which can flexibly adjust the ultrapure ammonia and the electronic grade ammonia water to meet the fluctuation of market price, thereby improving the economic benefit of enterprises.

[0007] Preferably, the electronic grade ammonia water preparation part comprises an electronic grade ammonia water washing tower, the middle and lower part inlet of the electronic grade ammonia water washing tower is connected with the third end of the first three-way joint, the upper part inlet of the electronic grade ammonia water washing tower is connected with the pure water storage tank, and the bottom of the electronic grade ammonia water washing tower is connected with the electronic grade ammonia water storage tank through the electronic ammonia water filtering storage tank.

[0008] Preferably, the liquid storage tank comprises a liquid storage tank shell, a liquid phase inlet is arranged in the middle part of the liquid storage tank shell, an overflow weir is arranged outside the liquid phase inlet and connected with the inner wall of the liquid storage tank shell, a first outlet is arranged on the liquid storage tank shell corresponding to the inside of the overflow weir, the first outlet is connected with the heavy component removal rectifying tower upper part heavy component removal rectifying tower reflux liquid inlet through a first valve, a second outlet is arranged on the liquid storage tank shell corresponding to the outside of the overflow weir, and the second outlet is connected with the ultrapure ammonia product storage tank through a second valve.

[0009] Preferably, the liquid storage tank is fixedly arranged at the top of the heavy component removal rectifying tower.

[0010] Preferably, the rectifying unit comprises a light component removal rectifying tower and a heavy component removal rectifying tower, the bottom liquid phase outlets of the light component removal rectifying tower and the heavy component removal rectifying tower are connected with the inlets of the composite reboiler respectively, the top gas phase outlets of the composite reboiler are connected with the lower part inlets of the light component removal rectifying tower and the heavy component removal rectifying tower respectively, and the bottom liquid phase outlet of the composite reboiler is connected with the industrial ammonia recovery tank.

[0011] Preferably, a first U-shaped pipe is arranged on the pipeline between the light component removal rectifying tower and the inlet of the composite reboiler, and a second U-shaped pipe is arranged on the pipeline between the heavy component removal rectifying tower and the inlet of the composite reboiler.

[0012] Preferably, the gas phase outlet at the top of the light component removal rectifying tower is connected with the light component removal rectifying tower reflux liquid through the second pipe passage of the composite condenser; a second three-way joint is arranged between the gas phase at the top of the light component removal rectifying tower and the second pipe passage of the composite condenser, and the third end of the second three-way joint is connected with the industrial ammonia recovery tank.

[0013] Preferably, a third valve is arranged between the first three-way joint and the first pipe passage of the composite condenser, and a fourth valve is arranged between the third end of the first three-way joint and the electronic grade ammonia water preparation part.

[0014] Preferably, a filter is arranged between the raw material storage tank and the rectifying unit.

[0015] Compared with the prior art, the utility model has the following advantages:

[0016] 1、The utility model discloses a production system of ultra -pure ammonia can realize two special gas products of ultra -pure ammonia and electronic grade ammonia water, to realize the production of ultra -pure ammonia and electronic grade ammonia water and satisfy the fluctuation of market price's characteristics, simplify electronic grade ammonia water's production process simultaneously, reduce production energy consumption.

[0017] 2、The utility model discloses electronic grade ammonia water with ultra -pure ammonia gas as raw material production can effectively guarantee product quality, and can make the production capacity of ultra -pure ammonia and electronic grade ammonia water realize 0 to 100 percent full load flexible regulation.

[0018] 3、The utility model discloses a composite condenser for double -channel heat exchanger, it has replaced traditional column -tube heat exchanger, with the characteristics of saving equipment investment, reducing equipment floor area and energy -conserving and loss -reducing, and it can reduce energy consumption by about 20 percent.

[0019] 4、The utility model discloses still use composite reboiler, can realize two rectifying column and one reboiler matching characteristics, thereby reduce the energy consumption loss of gas -liquid mass transfer heat transfer process, with the characteristics of reducing equipment floor area and energy -conserving and loss -reducing. BRIEF DESCRIPTION OF DRAWINGS

[0020] In order to more clearly illustrate the technical scheme in the embodiments of the utility model or prior art, the following will briefly introduce the drawings needed to be used in the embodiment or prior art description, obviously, the drawings in the following description only some embodiments of the utility model, for those skilled in the art, under the premise of not paying creative labor, still can obtain other drawings according to these drawings.

[0021] Figure 1 It is the structural schematic diagram of the utility model.

[0022] In the drawing: 1, raw material storage tank;2, filter;3, light removal rectifying column;4, heavy removal rectifying column;5, composite reboiler;6, composite condenser;7, liquid storage tank;8, electronic grade ammonia water washing tower;9, pure water storage tank;10, ultra -pure ammonia product storage tank;11, electronic ammonia water filter storage tank;12, electronic grade ammonia water storage tank;13, industrial ammonia recovery tank;14, overflow weir;15, first tee;16, second tee;17, first U-shaped pipe;18, second U-shaped pipe;19, first valve;20, second valve;21, third valve;22, fourth valve. DETAILED DESCRIPTION

[0023] Clearly, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0024] The technical scheme in the embodiments of the present application will be described clearly and completely in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application. Figure 1 Further, the electronic grade ammonia water preparation part includes an electronic grade ammonia water washing tower 8, the middle and lower part inlet of the electronic grade ammonia water washing tower 8 is connected with the third end of the first three-way pipe 15, the upper part inlet of the electronic grade ammonia water washing tower 8 is connected with the pure water storage tank 9, and the bottom of the electronic grade ammonia water washing tower 8 is connected with the electronic grade ammonia water storage tank 12 through the electronic ammonia water filtering storage tank 11.

[0025] Further, the electronic grade ammonia water preparation part includes an electronic grade ammonia water washing tower 8, the middle and lower part inlet of the electronic grade ammonia water washing tower 8 is connected with the third end of the first three-way pipe 15, the upper part inlet of the electronic grade ammonia water washing tower 8 is connected with the pure water storage tank 9, and the bottom of the electronic grade ammonia water washing tower 8 is connected with the electronic grade ammonia water storage tank 12 through the electronic ammonia water filtering storage tank 11.

[0026] Further, the liquid storage tank 7 includes a liquid storage tank shell, a liquid phase inlet is arranged in the middle part of the liquid storage tank shell, an overflow weir 14 connected with the inner wall of the liquid storage tank shell is arranged outside the liquid phase inlet, a first outlet is arranged in the liquid storage tank shell corresponding to the inside of the overflow weir 14, the first outlet is connected with the heavy fraction rectification tower 4 upper part heavy fraction rectification tower reflux liquid inlet through a first valve 19, a second outlet is arranged in the liquid storage tank shell corresponding to the outside of the overflow weir 14, and the second outlet is connected with the ultra-pure ammonia product storage tank 10 through a second valve 20.

[0027] Further, the liquid storage tank 7 is fixedly arranged at the top of the heavy fraction rectification tower 4.

[0028] Further, the rectification unit includes the light fraction rectification tower 3 and the heavy fraction rectification tower 4, the bottom liquid phase outlets of the light fraction rectification tower 3 and the heavy fraction rectification tower 4 are connected with the inlets of the composite reboiler 5 respectively, the top gas phase outlets of the composite reboiler 5 are connected with the lower inlets of the light fraction rectification tower 3 and the heavy fraction rectification tower 4 respectively, and the bottom liquid phase outlet of the composite reboiler 5 is connected with the industrial ammonia recovery tank 13.

[0029] Further, a first U-shaped pipe 17 is arranged on the pipeline between the light-removing rectifying tower 3 and the inlet of the composite reboiler 5, and a second U-shaped pipe 18 is arranged on the pipeline between the heavy-removing rectifying tower 4 and the inlet of the composite reboiler 5.

[0030] Further, the gas phase outlet at the top of the light-removing rectifying tower 3 is connected with the reflux liquid phase of the light-removing rectifying tower 3 through the second pipe passage of the composite condenser 6; a second three-way pipe 16 is arranged between the gas phase at the top of the light-removing rectifying tower 3 and the second pipe passage of the composite condenser 6, and the third end of the second three-way pipe 16 is connected with the industrial ammonia recovery tank 13.

[0031] Further, a third valve 21 is arranged between the first three-way pipe 15 and the first pipe passage of the composite condenser 6, and a fourth valve 22 is arranged between the third end of the first three-way pipe 15 and the electronic-grade ammonia water preparation part.

[0032] Further, a filter 2 is arranged between the raw material storage tank 1 and the rectifying unit.

[0033] The specific working process of the utility model is as follows:

[0034] Step one: the liquid ammonia raw material in the raw material storage tank 1 is preferentially purified by the filter 2 and enters the light removal rectification tower 3; the composition of the liquid ammonia raw material is methane, carbon dioxide, argon, nitrogen, moisture, etc.; the temperature of the raw material liquid is 22℃, the pressure is 1.0-1.5MpaG, it is saturated liquid, the molar fraction of liquid ammonia is ≥99%, and the index of liquid ammonia meets the index requirements in "Liquid Anhydrous Ammonia" GB / T536-2017. Step two: the gas phase after purification in step one enters the second three-way valve 16 through the gas phase outlet at the top of the light removal rectification tower 3, part of which enters the industrial ammonia recovery tank 13 for recovery; the other part enters the second tube passage of the composite condenser 6 to be condensed and liquefied, and after condensation and liquefaction, it is used as reflux liquid to enter the light removal rectification tower 3; the liquid phase after rectification enters the composite reboiler 5 through the liquid phase outlet at the bottom of the light removal rectification tower 3; the first U-shaped pipe 17 is arranged between the light removal rectification tower 3 and the composite reboiler 5 to prevent gas backflow; the composite condenser 6 is a double-channel high-efficiency heat exchanger, which has the characteristics of reducing energy consumption. Step three: the raw material in step two is vaporized in the composite reboiler 5, part of the vaporized gas enters the light removal rectification tower 3 through the gas phase outlet at the top of the composite reboiler 5 to provide a hot gas source for the light removal rectification tower 3; the other part of the vaporized gas enters the heavy removal rectification tower 4 for further rectification; the content of methane, carbon dioxide, argon and nitrogen in the light components of the gas phase outlet at the top of the composite reboiler 5 is ≤10ppb, and the molar fraction of liquid ammonia is ≥99.99%. Step four: the crude product in step three is further purified, and the purified rectification liquid enters the composite reboiler 5 through the tower kettle of the heavy removal rectification tower 4; the liquid in the composite reboiler 5 enters the industrial ammonia recovery tank 13 through the liquid phase outlet at the bottom of the composite reboiler 5 to recover and treat the residual liquid; the second U-shaped pipe 18 is arranged on the pipeline between the heavy removal rectification tower 4 and the inlet of the composite reboiler 5 to prevent gas backflow. Step five: the gas phase after purification in the heavy removal rectification tower 4 can be selected to enter the electronic grade ammonia water preparation part and / or the ultra-pure ammonia product storage tank 10; when producing ultra-pure ammonia products, the purified ultra-pure ammonia gas phase enters the first tube passage of the composite condenser 6 to be liquefied, and the liquefied ultra-pure liquid ammonia enters the overflow weir 14 of the liquid storage tank 7; the quality of the purified ultra-pure ammonia gas has reached 7N, and the product quality meets the index of "Ultra-pure Ammonia" T / CCGA 30001-2019.Step six: the ultra-pure liquid ammonia in the overflow weir 14 enters the de-heavy rectification tower 4 through the first valve 19 to provide reflux liquid for rectification; as the production continues, the ultra-pure liquid ammonia accumulates continuously, the ultra-pure liquid ammonia enters the liquid storage tank 7 through the overflow weir 14, the ultra-pure liquid ammonia in the liquid storage tank 7 enters the ultra-pure ammonia product storage tank 10 through the second valve 20; the liquid storage tank 7 is provided with an overflow weir 14, which can separate the reflux liquid and the product production liquid through the equipment structure, improve the stability of the product, and further enable the metal ions in the product to be in the overflow weir 14, so as to improve the quality of the ultra-pure liquid ammonia product. Step seven: the purified ultra-pure ammonia gas phase enters the electronic grade ammonia water washing tower 8, which is fully contacted and absorbed with the top spraying ultra-pure water in the electronic grade ammonia water washing tower 8 filler, and finally obtains the electronic grade ammonia water product in the electronic grade ammonia water washing tower 8, the electronic grade ammonia water product enters the electronic grade ammonia water storage tank 12 through the bottom of the electronic grade ammonia water washing tower 8 and the electronic ammonia water filtering storage tank 11. The required pure water for the top spraying is provided by the pure water storage tank 9; the electronic grade ammonia water meets the industry demand.

[0035] The basic principle, main features and advantages of the present application are shown and described above. It should be understood by those skilled in the art that the present application is not limited by the above examples, and the above examples and descriptions in the specification are only to illustrate the principles of the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the present application.

Claims

1. A plant for the co-production of ultra-pure ammonia and electronic grade aqueous ammonia, comprising a feedstock storage tank (1), an ultra-pure ammonia product storage tank (10) and an electronic grade aqueous ammonia storage tank (12), characterized in that: The raw material storage tank (1) is connected with the ultra-pure ammonia product storage tank (10) through a rectification unit, The rectification unit comprises a light-removing rectification tower (3) and a heavy-removing rectification tower (4), a gas phase outlet of the heavy-removing rectification tower (4) is connected with a first tube passage of a composite condenser (6) through a first three-way pipe (15), the first tube passage of the composite condenser (6) is connected with a liquid storage tank (7), and the liquid storage tank (7) is connected with a reflux liquid inlet of the heavy-removing rectification tower (4) and the ultra-pure ammonia product storage tank (10) respectively; A third end of the first three-way pipe (15) is connected with an electronic grade ammonia water preparation part and an electronic grade ammonia water storage tank (12).

2. A plant for co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 1, characterized in that: The electronic grade ammonia water preparation part comprises an electronic grade ammonia water washing tower (8), a middle and lower part inlet of the electronic grade ammonia water washing tower (8) is connected with the third end of the first three-way pipe (15), an upper part inlet of the electronic grade ammonia water washing tower (8) is connected with a pure water storage tank (9), and a bottom of the electronic grade ammonia water washing tower (8) is connected with the electronic grade ammonia water storage tank (12) through an electronic ammonia water filtering storage tank (11).

3. A plant for co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 1, characterized in that: The liquid storage tank (7) comprises a liquid storage tank shell, a liquid phase inlet is arranged in the middle of the liquid storage tank shell, an overflow weir (14) connected with an inner wall of the liquid storage tank shell is arranged outside the liquid phase inlet, a first outlet is arranged in the liquid storage tank shell corresponding to the inside of the overflow weir (14), the first outlet is connected with a heavy-removing rectification tower reflux liquid inlet in the upper part of the heavy-removing rectification tower (4) through a first valve (19), a second outlet is arranged in the liquid storage tank shell corresponding to the outside of the overflow weir (14), and the second outlet is connected with the ultra-pure ammonia product storage tank (10) through a second valve (20).

4. A plant for the co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 3, characterized in that: The liquid storage tank (7) is fixedly arranged at the top of the heavy-removing rectification tower (4).

5. A plant for co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 1, characterized in that: The rectification unit comprises the light-removing rectification tower (3) and the heavy-removing rectification tower (4), bottom liquid phase outlets of the light-removing rectification tower (3) and the heavy-removing rectification tower (4) are connected with inlets of a composite reboiler (5) respectively, a top gas phase outlet of the composite reboiler (5) is connected with lower part inlets of the light-removing rectification tower (3) and the heavy-removing rectification tower (4) respectively, and a bottom liquid phase outlet of the composite reboiler (5) is connected with an industrial ammonia recovery tank (13).

6. A plant for the co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 5, characterized in that: A first U-shaped pipe (17) is arranged on a pipeline between the light-removing rectification tower (3) and the inlet of the composite reboiler (5), and a second U-shaped pipe (18) is arranged on a pipeline between the heavy-removing rectification tower (4) and the inlet of the composite reboiler (5).

7. A plant for co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 5, characterized in that: A gas phase outlet at the top of the light-removing rectification tower (3) is connected with a heavy-removing rectification tower reflux liquid through a second tube passage of the composite condenser (6); a second three-way pipe (16) is arranged between the gas phase at the top of the light-removing rectification tower (3) and the second tube passage of the composite condenser (6), and a third end of the second three-way pipe (16) is connected with the industrial ammonia recovery tank (13).

8. A plant for the co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 7, characterized in that: A third valve (21) is arranged between the first three-way pipe (15) and the first tube passage of the composite condenser (6), and a fourth valve (22) is arranged between the third end of the first three-way pipe (15) and the electronic grade ammonia water preparation part.

9. A plant for co-production of ultra-pure ammonia and electronic grade aqueous ammonia according to claim 1, characterized in that: A filter (2) is arranged between the raw material storage tank (1) and the rectification unit.

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