CN216005233U - Production device suitable for electronic grade ammonia and ammonia water - Google Patents

Abstract

The utility model discloses a production device suitable for electronic grade ammonia and ammonia water, which relates to the technical field of chemical industry and comprises an evaporator, a gas-liquid separator, an adsorption device, a first rectifying device, a second rectifying device, a first washing device, a second washing device, an absorption device and a filtering device which are sequentially communicated; wherein, be equipped with the thermal coupling device between first rectifier unit and the second rectifier unit, second rectifier unit has top of the tower gas outlet, first import and second import, and the thermal coupling device has liquid ammonia import, hot gas export and liquid ammonia export, and the liquid ammonia export is linked together with first import, and first rectifier unit is linked together with the second import, and the top of the tower gas outlet is linked together with hot gas import, first washing device and ammonia storage device respectively. The production device in this application not only can be applicable to the production of electron level ammonia and electron level aqueous ammonia simultaneously, and has improved energy consumption utilization ratio, and then has reduced manufacturing cost.

Description

Production device suitable for electronic grade ammonia and ammonia water

Technical Field

The utility model relates to a chemical industry equipment technical field, concretely relates to apparatus for producing suitable for electron level ammonia and aqueous ammonia.

Background

With the development of the semiconductor industry, the requirements on the trace metal impurity content, the particle size and the number of particles, the anion impurity content and the like of wet electronic chemicals are more and more strict, and the market more and more needs more ultra-pure electronic grade chemicals and gases. At present, electronic-grade ammonia gas and electronic-grade ammonia water are main ultrapure chemical materials commonly used in the semiconductor industry and have important functions in the manufacturing industries of integrated circuits, LCDs and the like, wherein the electronic-grade ammonia gas is mainly used for cleaning, etching, doping and precipitating processes of chips, the electronic-grade ammonia water is mainly used for removing particles and organic matters attached to the surfaces of silicon wafers in the integrated circuit industry by using weak alkalinity of the electronic-grade ammonia water, and etching is performed on mixed liquid of silicon and cobalt metal ions commonly used and hydrogen peroxide; namely, the electronic-grade ammonia water is widely applied to the cleaning and etching process of the chip. However, although there are many methods for preparing electronic grade ammonia gas and electronic grade ammonia water, the preparation method and the related production apparatus in the prior art have single functionality, i.e. only electronic grade ammonia gas or electronic grade ammonia water can be produced singly, and it is difficult to apply to the preparation of electronic grade ammonia gas and electronic grade ammonia water at the same time. Meanwhile, the preparation method of electronic grade ammonia gas or electronic grade ammonia water still has the problem of high production cost caused by low energy consumption utilization rate in the rectification process.

SUMMERY OF THE UTILITY MODEL

1. Technical problem to be solved by the utility model

The production device to electron level ammonia or electron level aqueous ammonia among the prior art can't satisfy the technical problem who is applicable to the production of electron level ammonia and electron level aqueous ammonia simultaneously, the utility model provides a production device suitable for electron level ammonia and aqueous ammonia, it not only can be applicable to the production of electron level ammonia and electron level aqueous ammonia simultaneously, and energy consumption high-usage, low in production cost.

2. Technical scheme

In order to solve the above problem, the utility model provides a technical scheme does:

a production device suitable for electronic-grade ammonia gas and ammonia water comprises an evaporator, a gas-liquid separator, an adsorption device, a first rectification device, a second rectification device, a first washing device, a second washing device, an absorption device and a filtering device which are sequentially communicated; wherein, first rectifier unit with be equipped with the thermal coupling device between the second rectifier unit, the second rectifier unit has top of the tower gas outlet, first import and second import, the thermal coupling device has liquid ammonia import, hot gas outlet and liquid ammonia export, the liquid ammonia import with the bottom of first rectifier unit is linked together, hot gas import with the top of the tower gas outlet of second rectifier unit is linked together, hot gas export with the tower cauldron of first rectifier unit is linked together, the liquid ammonia export with the first import of second rectifier unit is linked together, first rectifier unit with the second import of second rectifier unit is linked together, the top of the tower gas outlet of second rectifier unit respectively with hot gas import, first washing device and ammonia storage device are linked together.

In the utility model, industrial-grade liquid ammonia to be treated is introduced into an evaporator to be evaporated at low pressure to obtain ammonia gas, then the ammonia gas enters a gas-liquid separator, substances such as moisture and large particles entrained in the ammonia gas are separated out by the gas-liquid separator, the ammonia gas treated by the gas-liquid separator enters an adsorption device, and the residual moisture, other gases and other impurities in the ammonia gas are further removed by the adsorption device, so that the ammonia gas is further purified; the ammonia gas treated by the adsorption device enters a first rectification device for rectification and purification, after rectification and purification, one part of liquid ammonia at the bottom of the first rectification device enters a thermal coupling device from a liquid ammonia inlet through a pipeline, the other part of liquid ammonia enters a second rectification device for rectification and purification again, the ammonia gas rectified and purified by the second rectification device is discharged from a tower top gas outlet and is divided into three parts, the first part of ammonia gas enters the thermal coupling device from a hot gas inlet through a pipeline, the second part of ammonia gas enters a first washing device, and the third part of ammonia gas is collected by an ammonia gas storage device to obtain ultra-pure electronic-grade ammonia gas; liquid ammonia treated by the first rectifying device entering from a liquid ammonia inlet exchanges heat with a first part of ammonia gas discharged from an air outlet at the top of the second rectifying device entering from a hot gas inlet in the thermal coupling device, and hot ammonia gas after heat exchange treatment enters a tower kettle of the first rectifying device from a hot gas outlet through a pipeline to supplement heat for the first rectifying device so as to provide heat load for the first rectifying device; liquid ammonia after heat exchange treatment enters the second rectifying device through a liquid ammonia outlet through a pipeline for reflux purification again, and cold load is provided for the second rectifying device; then, a second part of ammonia gas entering the first washing device is washed by ultrapure water with the resistivity larger than 18M omega cm, the ammonia gas treated by the first washing device enters the second washing device again, the ultrapure water with the resistivity larger than 18M omega cm is used for washing again, impurities, metal ions and the like in the ammonia gas are further washed and removed, a semi-finished product of ammonia water is obtained, the ammonia gas treated by the second washing device enters the absorption device, and the ultrapure water with the resistivity of 18M omega cm is used for absorption; and finally, filtering by a filtering device to obtain the ultrapure electronic-grade ammonia water.

Therefore, the utility model discloses a first rectifier unit with set up the thermal coupling device between the second rectifier unit, can effectively save the heat load of first rectifier unit and the cold load of second rectifier unit, improved the energy consumption utilization ratio of first rectifier unit and second rectifier unit greatly, the energy consumption is 60% of conventional rectification, greatly reduced manufacturing cost. Simultaneously, compare in prior art in the apparatus for producing of electron level ammonia gas or electron level aqueous ammonia, the utility model provides a production device can produce electron level ammonia gas and electron level aqueous ammonia alone, also can produce electron level ammonia gas and electron level aqueous ammonia simultaneously. Therefore, the utility model provides a production device not only can be applicable to the production of electron level ammonia and electron level aqueous ammonia simultaneously, and has improved energy consumption utilization ratio, and then reduction in production cost.

Optionally, the evaporator further comprises a filter having an inlet and an outlet, the inlet of the filter is used for receiving industrial-grade liquid ammonia, and the outlet of the filter is communicated with the evaporator.

Optionally, the gas-liquid separator has a third inlet, a gas outlet and a return port, the evaporator is respectively communicated with the third inlet and the return port, and the gas outlet is communicated with the adsorption device.

Optionally, the gas purification device further comprises a gas purifier, the gas purifier is provided with a gas inlet and a gas outlet, the gas inlet of the gas purifier is communicated with the adsorption device, and the gas outlet of the gas purifier is communicated with the first rectification device.

Optionally, an air outlet at the top of the second rectifying device is communicated with the hot gas inlet through a pipeline, and a thermal coupling power device is arranged on the pipeline.

Optionally, a heat exchange device is arranged outside the second rectification device, one end of the heat exchange device is communicated with the bottom of the second rectification device, and the other end of the heat exchange device is communicated with the tower kettle of the second rectification device.

Optionally, a first circulating device is arranged outside the first washing device, one end of the first circulating device is communicated with the bottom of the first washing device, and the other end of the first circulating device is communicated with the middle upper part of the first washing device.

Optionally, a second circulation device is arranged outside the second washing device, one end of the second circulation device is communicated with the bottom of the second washing device, and the other end of the second circulation device is communicated with the middle upper part of the second washing device.

Optionally, a third circulating device is arranged between the absorption device and the filtering device, one end of the third circulating device is communicated with the absorption device, and the other end of the third circulating device is communicated with the filtering device.

Optionally, a return pipeline is arranged between the absorption device and the filtering device.

3. Advantageous effects

Adopt the technical scheme provided by the utility model, compare with prior art, have following beneficial effect:

(1) the embodiment of the application provides a production device suitable for electron level ammonia and aqueous ammonia, simple structure through first rectifier unit with set up the thermal coupling device between the second rectifier unit, can effectively save the heat load of first rectifier unit and the cold load of second rectifier unit, improved the energy consumption utilization ratio of first rectifier unit and second rectifier unit greatly, the energy consumption is 60% of conventional rectification, greatly reduced manufacturing cost. Simultaneously, compare in prior art in the apparatus for producing of electron level ammonia gas or electron level aqueous ammonia, apparatus for producing in this application can produce electron level ammonia gas and electron level aqueous ammonia alone, also can produce electron level ammonia gas and electron level aqueous ammonia simultaneously. Therefore, the production device in the application not only can be simultaneously suitable for the production of electronic grade ammonia and electronic grade ammonia water, but also improves the energy consumption utilization rate and further reduces the production cost.

(2) The apparatus for producing suitable for electron level ammonia and aqueous ammonia that this application embodiment provided sets up impurity and large granule material that the filter is used for filtering in the industrial level liquid ammonia, is favorable to improving the purification effect of follow-up device.

(3) The apparatus for producing suitable for electron level ammonia and aqueous ammonia that this application embodiment provided sets up gas purifier and can further purify the ammonia, improves the purification degree of ammonia.

(4) The apparatus for producing suitable for electron level ammonia and aqueous ammonia that this application embodiment provided is convenient for concentrate the first part ammonia in the second rectifier unit to the thermal coupling device in through setting up thermal coupling power device.

(5) According to the production device suitable for electronic-grade ammonia gas and ammonia water, impurities such as metal ions in the ammonia gas washed by the first washing device can be further washed in the filler by arranging the first circulating device, and the ammonia gas is circularly washed to obtain the ammonia water with high purity; and a second circulating device is arranged, so that impurities such as metal ions in the ammonia gas washed by the second washing device can be further washed in the filler, the ammonia gas is circularly washed, and the purity of the obtained ammonia water is further improved.

(6) The apparatus for producing suitable for electron level ammonia and aqueous ammonia that this application embodiment provided through setting up third circulating device, can effectively get rid of in absorbing device or the impurity that introduces in the circulation process, further improves the purity of aqueous ammonia.

Drawings

Fig. 1 is a schematic structural diagram of a production device suitable for electronic grade ammonia and ammonia water provided by the embodiment of the utility model.

Detailed Description

For a further understanding of the present invention, reference will be made to the following detailed description taken in conjunction with the accompanying drawings and examples.

The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and are not limiting of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings. The utility model discloses in words such as first, second, be for the description the utility model discloses a technical scheme is convenient and set up, and does not have specific limiting action, is general finger, right the technical scheme of the utility model does not constitute limiting action. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art. The technical solutions in the same embodiment and between the technical solutions in different embodiments can be arranged and combined to form a new technical solution without contradiction or conflict, which is all within the scope of the present invention.

Example 1

With reference to fig. 1, the embodiment provides a production apparatus suitable for electronic grade ammonia gas and ammonia water, which includes an evaporator 2, a gas-liquid separator 3, an adsorption apparatus 4, a first rectification apparatus 6, a second rectification apparatus 8, a first washing apparatus 14, a second washing apparatus 15, an absorption apparatus 16, and a filtering apparatus 17, which are sequentially communicated; wherein a thermal coupling device 9 is arranged between the first rectifying device 6 and the second rectifying device 8, the second rectifying means 8 has an overhead gas outlet 22, a first inlet 23 and a second inlet 24, the thermal coupling device 9 has a liquid ammonia inlet 10, a hot gas inlet 11, a hot gas outlet 13 and a liquid ammonia outlet 12, the liquid ammonia inlet 10 is communicated with the bottom of the first rectifying device 6, the hot gas inlet 11 is communicated with the top gas outlet 22 of the second rectifying device 8, the hot gas outlet 13 is communicated with the tower kettle of the first rectifying device 6, the liquid ammonia outlet 12 is communicated with the first inlet 23 of the second rectifying device 8, the first rectifying device 6 is communicated with a second inlet 24 of the second rectifying device 8, and an air outlet 22 at the top of the second rectifying device 8 is respectively communicated with the hot air inlet 11, the first washing device 14 and an ammonia gas storage device (not shown in the figure).

In the application, industrial-grade liquid ammonia to be treated is introduced into an evaporator 2 to be evaporated at low pressure to obtain ammonia gas, then the ammonia gas enters a gas-liquid separator 3, substances such as moisture and large particles entrained in the ammonia gas are separated out through the gas-liquid separator 3, the ammonia gas treated by the gas-liquid separator 3 enters an adsorption device 4, and the residual moisture, other gases and other impurities in the ammonia gas are further removed through the adsorption device 4, so that the ammonia gas is further purified; the ammonia gas treated by the adsorption device 4 enters a first rectification device 6 for rectification and purification, after rectification and purification, one part of liquid ammonia at the bottom of the first rectification device 6 enters a thermal coupling device 9 from a liquid ammonia inlet 10 through a pipeline, the other part of liquid ammonia enters a second rectification device 8 for rectification and purification again, the ammonia gas rectified and purified by the second rectification device 8 is discharged from a tower top gas outlet 22 and is divided into three parts, the first part of ammonia gas enters the thermal coupling device 9 from a hot gas inlet 11 through a pipeline, the second part of ammonia gas enters a first washing device 14, and the third part of ammonia gas is collected by an ammonia gas storage device to obtain ultra-pure electronic-grade ammonia gas, wherein the main content of the ammonia gas exceeds 99.99999 percent (greater than 7N); liquid ammonia treated by the first rectifying device 6 and entering from a liquid ammonia inlet 10 exchanges heat with a first part of ammonia gas discharged from an air outlet 22 at the top of the second rectifying device 8 and entering from a hot gas inlet 11 in a thermal coupling device 9, and hot ammonia gas after heat exchange treatment enters a tower kettle of the first rectifying device 6 from a hot gas outlet 13 through a pipeline to supplement heat for the first rectifying device 6, so that heat load is provided for the first rectifying device 6; the liquid ammonia after heat exchange treatment enters the second rectifying device 8 through a liquid ammonia outlet 12 through a pipeline for reflux purification again, and a cooling load is provided for the second rectifying device 8; then, a second part of ammonia gas entering the first washing device 14 is washed by ultrapure water with the resistivity larger than 18M Ω & cm, the ammonia gas treated by the first washing device 14 enters the second washing device 15 again, and is washed again by ultrapure water with the resistivity larger than 18M Ω & cm, impurities, metal ions and the like in the ammonia gas are further washed and removed, a semi-finished product of ammonia water is obtained, the ammonia gas treated by the second washing device 15 enters the absorption device 16, and is absorbed by ultrapure water with the resistivity of 18M Ω & cm; finally, the ultra-pure electronic grade ammonia water is obtained by filtering through a filtering device 17.

Therefore, the thermal coupling device 9 is arranged between the first rectifying device 6 and the second rectifying device 8, so that the heat load of the first rectifying device 6 and the cold load of the second rectifying device 8 can be effectively saved, the energy consumption utilization rate of the first rectifying device 6 and the second rectifying device 8 is greatly improved, the energy consumption is 60% of the conventional rectification, and the production cost is greatly reduced. Simultaneously, compare in prior art in the apparatus for producing of electron level ammonia gas or electron level aqueous ammonia, apparatus for producing in this application can produce electron level ammonia gas and electron level aqueous ammonia alone, also can produce electron level ammonia gas and electron level aqueous ammonia simultaneously. Therefore, the production device in the application not only can be simultaneously suitable for the production of electronic grade ammonia and electronic grade ammonia water, but also improves the energy consumption utilization rate and further reduces the production cost.

In practical application, the top of the first rectification device 6 is provided with a vent pipeline 32. The first rectifying device 6 comprises a tower top condenser, a filling device and a tower bottom reboiler, wherein the tower top condenser adopts a mechanical polishing tubular heat exchanger, the tower top condenser is connected with the vent pipeline 32, the vent pipeline 32 is used for being connected with outside air, so that redundant gas in the tower top condenser can be conveniently discharged in time, and the normal use of the first rectifying device 6 is ensured; the tower bottom reboiler is used for providing heat for the rectifying device.

Example 2

With reference to fig. 1, the apparatus for producing electronic-grade ammonia gas and ammonia water of the present embodiment further includes a filter 1, compared with the technical solution of embodiment 1, where the filter 1 has an inlet and an outlet, the inlet of the filter 1 is used for receiving industrial-grade ammonia water, and the outlet of the filter 1 is communicated with the evaporator 2. Set up impurity and large granule material that filter 1 is used for filtering in the industrial-grade liquid ammonia, be favorable to improving the purification effect of follow-up device.

Example 3

With reference to fig. 1, in the production apparatus for electronic-grade ammonia gas and ammonia water of the present embodiment, compared with the technical solution of embodiment 1, the gas-liquid separator 3 has a third inlet 28, a gas outlet 33 and a reflux port 29, the evaporator 2 is respectively communicated with the third inlet 28 and the reflux port 29, and the gas outlet 33 is communicated with the adsorption device 4.

Gaseous ammonia gas treated by the evaporator 2 enters the gas-liquid separator 3 through the third inlet 28 through a pipeline, liquid separated by the gas-liquid separator 3 returns to the evaporator 2 again through the corresponding return opening 29 and the return pipe 31 for secondary evaporation treatment, and recycling of materials is realized; the gas separated by the gas-liquid separator 3 is introduced into the adsorption apparatus 4 through the gas outlet 33.

Example 4

With reference to fig. 1, the production apparatus for electronic-grade ammonia gas and ammonia water of this embodiment further includes a gas purifier 5, the gas purifier 5 has a gas inlet and a gas outlet, the gas inlet of the gas purifier 5 is communicated with the adsorption device 4, and the gas outlet of the gas purifier 5 is communicated with the first rectification device 6, compared with the technical solutions of embodiments 1 and 2. This setting can further purify the ammonia, improves the purification degree of ammonia.

In practice, membranes of different particle sizes are provided in the gas purifier 5, and generally, the smaller the particle size, the smaller the size of the particles to be removed, and the greater the probability of removing particles exceeding this particle size, the less the ammonia gas as an impurity. In the embodiment, the grain size of the film is 10-30nm, and in practical application, such as films of 30nm and 10nm, the arrangement can effectively remove impurities in the ammonia gas and improve the purity of the ammonia gas.

Example 5

With reference to fig. 1, the apparatus for producing electronic grade ammonia gas and ammonia water according to this embodiment can be improved as follows compared with the technical solution of embodiment 1: and the tower top air outlet 22 of the second rectifying device 8 is communicated with the hot air inlet 11 through a pipeline, and the pipeline is provided with a thermal coupling power device 7. The concentration of the first portion of ammonia gas in second rectification means 8 into thermal coupling means 9 is facilitated by the provision of thermal coupling motive means 7.

Example 6

With reference to fig. 1, the apparatus for producing electronic grade ammonia gas and ammonia water according to this embodiment can be improved as follows compared with the technical solution of embodiment 1: a heat exchange device 18 is arranged on the outer side of the second rectifying device 8, one end of the heat exchange device 18 is communicated with the tower bottom of the second rectifying device 8, and the other end of the heat exchange device 18 is communicated with the tower kettle of the second rectifying device 8. The heat exchange device 18 can supplement the heat for the second rectifying device 8.

Example 7

With reference to fig. 1, the apparatus for producing electronic grade ammonia gas and ammonia water according to this embodiment can be improved as follows compared with the technical solution of embodiment 1: a first circulating device 19 is arranged outside the first washing device 14, one end of the first circulating device 19 is communicated with the bottom of the first washing device 14, and the other end of the first circulating device 19 is communicated with the middle upper part of the first washing device 14.

In practical applications, a washing filler area is arranged in the first washing device 14, and the washing filler area is arranged between an inlet and an outlet of the first washing device 14. One end of the first circulating device 19 is communicated with the bottom of the first washing device 14 through a pipeline, and a circulating pump is arranged on the pipeline. In this embodiment, the first circulation device 19 is arranged to further wash impurities, such as metal ions, in the ammonia gas washed by the first washing device 14 in the filler, and perform a circulation washing process on the ammonia gas to obtain ammonia water with higher purity.

In practical applications, the first circulating device 19 is further connected to a first condensing device for absorbing heat in the gas, and the temperature of the whole circulating system is controlled to be constant by cooling the whole circulating system, so as to prevent the temperature of the system from being too high.

Example 8

With reference to fig. 1, the apparatus for producing electronic grade ammonia gas and ammonia water according to this embodiment can be improved as follows compared with the technical solution of embodiment 1: a second circulating device 20 is arranged outside the second washing device 15, one end of the second circulating device 20 is communicated with the bottom of the second washing device 15, and the other end of the second circulating device 20 is communicated with the middle upper part of the second washing device 15.

The structure of the second circulating device 20 is the same as that of the first circulating device 19, and the second circulating device 20 is arranged to further wash impurities such as metal ions in the ammonia gas washed by the second washing device 15 in the filler, and perform circulating washing treatment on the ammonia gas, so as to further improve the purity of the obtained ammonia water. In practice, the first washing device 14 and the second washing device 15 are respectively provided with a first ultrapure water inlet 25 and a second ultrapure water inlet 26.

Example 9

With reference to fig. 1, the apparatus for producing electronic grade ammonia gas and ammonia water according to this embodiment can be improved as follows compared with the technical solution of embodiment 1: a third circulating device is arranged between the absorption device 16 and the filtering device 17, one end of the third circulating device is communicated with the absorption device 16, and the other end of the third circulating device is communicated with the filtering device 17. The third circulating device can effectively remove impurities introduced in the absorption device 16 or in the circulating process, and further improve the purity of the ammonia water.

Example 10

With reference to fig. 1, compared with the technical solution of embodiment 9, the apparatus for producing electronic grade ammonia gas and ammonia water of this embodiment can be improved as follows: a return line 30 is provided between the absorption device 16 and the filter device 17. The ammonia water discharged from the filtering device 17 can enter the absorption device 16 and the third circulating device again through the return pipe 30, so that impurities possibly existing in the circulating process can be further removed, and the purity of the electronic-grade ammonia water can be further improved.

In practical application, the second washing device 15 is connected to the absorption device 16 through a pipeline, the pipeline is provided with an ultrapure water inlet 27, one end of the backflow pipeline 30 is connected to the absorption device 16 through the pipeline, the other end of the backflow pipeline is connected to the filtering device 17, and the connection between the backflow pipeline 30 and the pipeline is located between the ultrapure water inlet 27 and the absorption device 16. The arrangement can effectively utilize ultrapure water to further purify the ammonia water circulated and refluxed.

Meanwhile, the production method suitable for electronic grade ammonia gas and ammonia water comprises the following steps:

(1) evaporating industrial-grade liquid ammonia serving as a raw material to obtain ammonia gas;

(2) carrying out gas-liquid separation treatment on the ammonia gas obtained in the step (1), removing residual moisture and large-particle impurities in the ammonia gas, and further purifying through adsorption treatment;

(3) rectifying and purifying the ammonia gas treated in the step (2) by a first rectifying device;

(4) sending a part of the liquid ammonia at the bottom of the first rectifying device rectified and purified in the step (3) into a second rectifying device for rectification and purification again, and sending the other part of the liquid ammonia into a thermal coupling device;

(5) after rectification and purification are carried out again in the second rectifying device in the step (4), ammonia gas discharged from the top of the second rectifying device is divided into three parts for treatment, and the first part of ammonia gas enters the thermal coupling device and carries out heat exchange treatment with the liquid ammonia sent into the thermal coupling device in the step (3); the second part of ammonia is treated by the next procedure; collecting a third part of ammonia gas to obtain ultra-pure electronic grade ammonia gas;

(6) and (5) sequentially washing, absorbing and filtering the second part of ammonia gas in the step (5) to obtain the ultrapure electronic grade ammonia water.

This application through first rectifier unit 6 with set up thermal coupling device 9 between the second rectifier unit 8 and carry out the processing of thermal coupling technology, can effectively save the heat load of first rectifier unit 6 and the cold load of second rectifier unit 8, improved the energy consumption utilization ratio of first rectifier unit 6 and second rectifier unit 8 greatly, the energy consumption is 60% of conventional rectification, greatly reduced manufacturing cost. Meanwhile, compared with a production method of electronic-grade ammonia gas or electronic-grade ammonia water in the prior art, the production method in the application can be used for producing the electronic-grade ammonia gas and the electronic-grade ammonia water independently and can also be used for producing the electronic-grade ammonia gas and the electronic-grade ammonia water simultaneously. Therefore, the production method in the application can be simultaneously suitable for the production of electronic grade ammonia gas and electronic grade ammonia water, the energy consumption utilization rate is improved, and the production cost is further reduced.

In practical application, in step (4), the liquid ammonia at the bottom of the first rectification device, wherein 1/4 of the liquid ammonia is sent to the second rectification device for rectification and purification again, 3/4 of the liquid ammonia is sent to the thermal coupling device.

In the step (5), the ratio of the amount of the first part of ammonia gas to the ammonia gas discharged from the top of the second rectifying device is 3/4, and the ratio of the amount of the second part of ammonia gas to the ammonia gas discharged from the top of the second rectifying device is 0-1/4; the proportion of the third part of ammonia gas to the ammonia gas discharged from the top of the second rectifying device is 0-1/4, and the specific proportion value of the proportion of the second part of ammonia gas to the ammonia gas discharged from the top of the second rectifying device to the proportion of the third part of ammonia gas to the ammonia gas discharged from the top of the second rectifying device is determined according to whether the ammonia gas and the ammonia water are produced simultaneously.

In practical application, step (1) is preceded by a filtration treatment of industrial-grade liquid ammonia as raw material. And (3) before the step (3), performing gas purification treatment on the ammonia gas subjected to adsorption treatment in the step (2), wherein a plurality of membranes with different particle sizes are adopted in the gas purification treatment, and the particle size of each membrane is 10-30 nm. The washing in the step (6) includes a first washing treatment and a second washing treatment in which both of the first washing treatment and the second washing treatment are circularly washed with ultrapure water having a resistivity of more than 18 M.OMEGA.cm; in the absorption treatment in the step (6), absorption was performed using ultrapure water having a resistivity of 18 M.OMEGA.. cm.

The present invention and its embodiments have been described above schematically, and the description is not limited thereto, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching of the present invention, without departing from the inventive spirit of the present invention, the person skilled in the art should also design the similar structural modes and embodiments without creativity to the technical solution, and all shall fall within the protection scope of the present invention.

Claims (10)

1. A production device suitable for electronic-grade ammonia gas and ammonia water is characterized by comprising an evaporator, a gas-liquid separator, an adsorption device, a first rectifying device, a second rectifying device, a first washing device, a second washing device, an absorption device and a filtering device which are sequentially communicated; wherein, first rectifier unit with be equipped with the thermal coupling device between the second rectifier unit, the second rectifier unit has top of the tower gas outlet, first import and second import, the thermal coupling device has liquid ammonia import, hot gas outlet and liquid ammonia export, the liquid ammonia import with the bottom of first rectifier unit is linked together, hot gas import with the top of the tower gas outlet of second rectifier unit is linked together, hot gas export with the tower cauldron of first rectifier unit is linked together, the liquid ammonia export with the first import of second rectifier unit is linked together, first rectifier unit with the second import of second rectifier unit is linked together, the top of the tower gas outlet of second rectifier unit respectively with hot gas import, first washing device and ammonia storage device are linked together.

2. The apparatus for the production of ammonia and ammonia water of electronic grade according to claim 1, further comprising a filter having an inlet for receiving liquid ammonia of technical grade and an outlet, the outlet of said filter being in communication with said evaporator.

3. The apparatus for producing electronic grade ammonia gas and ammonia water as defined in claim 1, wherein the gas-liquid separator has a third inlet, a gas outlet and a return port, the evaporator is respectively communicated with the third inlet and the return port, and the gas outlet is communicated with the adsorption device.

4. The apparatus for producing ammonia and ammonia water in electronic grade according to claim 1 or 2, further comprising a gas purifier, wherein the gas purifier has a gas inlet and a gas outlet, the gas inlet of the gas purifier is communicated with the adsorption device, and the gas outlet of the gas purifier is communicated with the first rectification device.

5. The apparatus for producing electronic grade ammonia gas and ammonia water as defined in claim 1, wherein the outlet of the second rectifying device is connected to the hot gas inlet via a pipeline, and the pipeline is provided with a thermal coupling power device.

6. The production device for electronic-grade ammonia gas and ammonia water as claimed in claim 1, wherein a heat exchange device is arranged outside the second rectification device, one end of the heat exchange device is communicated with the bottom of the second rectification device, and the other end of the heat exchange device is communicated with the bottom of the second rectification device.

7. The apparatus for producing electronic grade ammonia gas and ammonia water as defined in claim 1, wherein a first circulation device is disposed outside the first scrubber, one end of the first circulation device is connected to the bottom of the first scrubber, and the other end of the first circulation device is connected to the middle upper part of the first scrubber.

8. The apparatus for producing electronic grade ammonia gas and ammonia water as defined in claim 1, wherein a second circulation device is provided outside the second scrubber, one end of the second circulation device is connected to the bottom of the second scrubber, and the other end of the second circulation device is connected to the middle upper part of the second scrubber.

9. The apparatus for the production of electronic grade ammonia gas and ammonia water as defined in claim 1, wherein a third circulating device is provided between the absorption device and the filtering device, one end of the third circulating device is connected to the absorption device, and the other end of the third circulating device is connected to the filtering device.

10. The apparatus for the production of electronic grade ammonia and aqua ammonia according to claim 9, wherein a return line is provided between the absorption device and the filtration device.

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