Chlorine purification device

Abstract

The chlorine purification device comprises a raw material tank, a vaporizer, a heavy component removal tower, a light component removal tower, a condenser, a reboiler and a finished product tank. The raw material tank is used for storing untreated liquid chlorine, the liquid chlorine enters the vaporizer for heat exchange to obtain chlorine, the chlorine enters the heavy component removal tower for rectification separation, and trace water, nitrogen trichloride, metal ions and other heavy components in the chlorine are discharged from a tower kettle of the heavy component removal tower in the rectification separation process; the chlorine after heavy component removal flows into a light component removal tower after being treated by a first condenser, oxygen, nitrogen, argon, hydrogen, carbon monoxide, carbon dioxide and hydrocarbon gases are discharged by the light component removal tower and a second condenser, and the generated chlorine enters a finished product tank to be stored for later use. Chlorine can be purified by using a relatively simple process, and environmental pollution cannot be caused in the purification process.

Description

Technical Field

[0001] The present application relates to the field of chlorine treatment, and in particular to a chlorine purification device. Background Art

[0002] Electronic grade chlorine is one of the important raw materials for my country's semiconductor and optoelectronic industries, and is a type of electronic special gas. Electronic grade products are mainly used in large-scale integrated circuits, liquid crystal screens, optoelectronic semiconductors, optical fibers, solar polycrystalline silicon cells, solar thin film cells and other fields. Electronic grade chlorine is mainly used in dry etching, optical fibers, thermal oxidation and crystal growth in the electronics industry. Dry etching, also known as dry etching, refers to a gas-solid reaction. The gas phase products mainly include GaCl 2 、AsCl 2 When using chlorine for plasma etching, 5% high-purity chlorine plus 95% helium are usually used.

[0003] The preparation methods of electronic-grade chlorine are mainly adsorption and distillation. Showa Denko's electronic-grade chlorine adopts photolysis adsorption distillation, which first uses a special light source to decompose nitrogen and chlorine, then removes part of the water in the chlorine by adsorption, and then removes the remaining impurities by distillation. The existing technology usually adopts the distillation process of electronic-grade chlorine, which passes through multiple de-heavy and de-light distillation towers. The number of equipment used in the overall process is large, resulting in high energy consumption in the process; or the adsorption distillation process is adopted. This process uses silicon tetrafluoride as an adsorbent to absorb moisture, and then the chlorine is de-lightened and de-heaved. When silicon tetrafluoride is used as an adsorbent, it has a short service life and a large amount of consumption, which easily pollutes the environment. Utility Model Content

[0004] In view of this, the present application proposes a chlorine purification device, which can use a relatively simple process to purify chlorine and will not cause environmental pollution during the purification process.

[0005] According to one aspect of the present application, a chlorine gas purification device is provided, comprising: a raw material tank, a vaporizer, a heavy removal tower, a light removal tower, a condenser, a reboiler and a finished product tank.

[0006] There are two condensers, namely the first condenser and the second condenser; there are two reboilers, namely the first reboiler and the second reboiler; the outlet end of the raw material tank is connected to the inlet end of the vaporizer by a pipeline, and the outlet end of the vaporizer is connected to the inlet end of the de-weighting tower by a pipeline; the de-weighting tower is connected to the first reboiler in a loop, the de-weighting tower is connected to the first condenser in a loop, and the outlet end of the first condenser is connected to the inlet end of the secondary de-lighting tower by a pipeline; the de-lighting tower is connected to the second reboiler in a loop, the de-lighting tower and the second condenser in a loop, and the outlet end of the de-lighting tower is connected to the finished product tank by a pipeline.

[0007] In one possible implementation, the vaporizer is connected to the first inlet of the de-weighting tower by a pipeline; the first outlet of the de-weighting tower and the inlet end of the first reboiler are connected by a pipeline, and the outlet end of the first reboiler and the second inlet of the de-weighting tower are connected by a pipeline; the second outlet of the de-weighting tower and the inlet end of the first condenser are connected by a pipeline, the first outlet of the first condenser and the third inlet of the de-weighting tower are connected by a pipeline, and the second outlet of the first condenser and the first inlet of the light-removing tower are connected by a pipeline.

[0008] In one possible implementation, the first outlet of the light-removal tower and the inlet end of the second reboiler are connected by a pipeline, the outlet end of the second reboiler and the second inlet of the light-removal tower are connected by a pipeline; the second outlet of the light-removal tower and the inlet end of the second condenser are connected by a pipeline, the outlet end of the second condenser and the third inlet of the light-removal tower are connected by a pipeline; the third outlet of the light-removal tower and the inlet end of the finished product tank are connected by a pipeline.

[0009] In a possible implementation, a prepurifier is further included, which is arranged between the vaporizer and the de-weighting tower; the outlet end of the vaporizer is connected to the inlet end of the prepurifier by a pipeline, and the outlet end of the prepurifier is connected to the inlet end of the de-weighting tower by a pipeline.

[0010] In one possible implementation, a third condenser is further included, which is arranged between the light-removal tower and the finished product tank; a pipeline is connected between the third outlet of the light-removal tower and the inlet end of the third condenser, and a pipeline is connected between the outlet end of the third condenser and the inlet end of the finished product tank.

[0011] In one possible implementation, the first inlet of the deweighting tower is arranged at the middle position in the height direction of the deweighting tower, the second inlet of the deweighting tower is arranged at a height lower than the first inlet of the deweighting tower, and the third inlet of the deweighting tower is arranged at a height higher than the first inlet of the deweighting tower.

[0012] In a possible implementation, the first outlet of the deweighting tower is arranged at the bottom of the deweighting tower, and the second outlet of the deweighting tower is arranged at the top of the deweighting tower.

[0013] In one possible implementation, the first inlet of the de-lightness tower is arranged at the middle position in the height direction of the de-lightness tower, the second inlet of the de-lightness tower is arranged at a height lower than the first inlet of the de-lightness tower, and the third inlet of the de-lightness tower is arranged at a height higher than the first inlet of the de-lightness tower.

[0014] In a possible implementation, the first outlet of the lightness removal tower is arranged at the top of the lightness removal tower, and the second outlet and the third outlet of the lightness removal tower are both arranged at the bottom of the lightness removal tower.

[0015] The beneficial effects of the present application are as follows: the raw material tank is used to store untreated liquid chlorine, the liquid chlorine enters the vaporizer for heat exchange to obtain chlorine, the chlorine enters the de-weighting tower for distillation separation, and during the distillation separation process, trace amounts of water, nitrogen trichloride and metal ions and other heavy components in the chlorine are discharged from the de-weighting tower kettle, the de-weighted chlorine flows into the de-lighting tower after the gas phase is treated by the first condenser, the de-lighting tower and the second condenser discharge oxygen, nitrogen, argon, hydrogen, carbon monoxide, carbon dioxide and hydrocarbon gases, and the generated chlorine enters the finished product tank for storage and standby. According to a chlorine purification device of the present application, a relatively simple process can be used to complete the purification of chlorine, and no environmental pollution will be caused during the purification process.

[0016] Other features and aspects of the present application will become apparent from the following detailed description of exemplary embodiments with reference to the attached drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate exemplary embodiments, features, and aspects of the present application and, together with the description, serve to explain the principles of the present application.

[0018] Figure 1 A connection diagram of a chlorine purification device according to an embodiment of the present application is shown. DETAILED DESCRIPTION

[0019] Various exemplary embodiments, features and aspects of the present application will be described in detail below with reference to the accompanying drawings. The same reference numerals in the accompanying drawings represent elements with the same or similar functions. Although various aspects of the embodiments are shown in the accompanying drawings, the drawings are not necessarily drawn to scale unless otherwise specified.

[0020] Among them, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application or simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0021] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0022] The word “exemplary” is used exclusively herein to mean “serving as an example, example, or illustration.” Any embodiment described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments.

[0023] In addition, in order to better illustrate the present application, numerous specific details are given in the following specific embodiments. It should be understood by those skilled in the art that the present application can also be implemented without certain specific details. In some examples, methods, means, components and circuits well known to those skilled in the art are not described in detail in order to highlight the subject matter of the present application.

[0024] like Figure 1 As shown, the chlorine gas purification device includes: a raw material tank 100, a vaporizer 200, a heavy removal tower 300, a light removal tower 400, a condenser, a reboiler and a finished product tank 700.

[0025] There are two condensers, namely the first condenser 510 and the second condenser 520; there are two reboilers, namely the first reboiler 610 and the second reboiler 620; the outlet end of the raw material tank 100 is connected to the inlet end of the vaporizer 200 by a pipeline, and the outlet end of the vaporizer 200 is connected to the inlet end of the de-weighting tower 300 by a pipeline; the de-weighting tower 300 is loop-connected to the first reboiler 610, the de-weighting tower 300 is loop-connected to the first condenser 510, and the outlet end of the first condenser 510 is connected to the inlet end of the light-removing tower 400 by a pipeline; the light-removing tower 400 is loop-connected to the second reboiler 620, the light-removing tower 400 and the second condenser 520 are loop-connected, and the outlet end of the light-removing tower 400 is connected to the finished product tank 700 by a pipeline.

[0026] In one possible implementation, the vaporizer 200 is connected to the first inlet of the de-weighting tower 300 by a pipeline; the first outlet of the de-weighting tower 300 is connected to the inlet end of the first reboiler 610 by a pipeline, and the outlet end of the first reboiler 610 is connected to the second inlet of the de-weighting tower 300 by a pipeline; the second outlet of the de-weighting tower 300 is connected to the inlet end of the first condenser 510 by a pipeline, the first outlet of the first condenser 510 is connected to the third inlet of the de-weighting tower 300 by a pipeline, and the second outlet of the first condenser 510 is connected to the first inlet of the light-removing tower 400 by a pipeline.

[0027] In one possible implementation, the first outlet of the de-lightening tower 400 is connected to the inlet end of the second reboiler 620 by a pipeline, and the outlet end of the second reboiler 620 is connected to the second inlet of the de-lightening tower 400 by a pipeline; the second outlet of the de-lightening tower 400 is connected to the inlet end of the second condenser 520 by a pipeline, and the outlet end of the second condenser 520 is connected to the third inlet of the de-lightening tower 400 by a pipeline; the third outlet of the de-lightening tower 400 is connected to the inlet end of the finished product tank 700 by a pipeline.

[0028] In a possible implementation, a pre-purifier 800 is further included, and the pre-purifier 800 is arranged between the vaporizer 200 and the de-weighting tower 300; the outlet end of the vaporizer 200 is connected to the inlet end of the pre-purifier 800 by a pipeline, and the outlet end of the pre-purifier 800 is connected to the inlet end of the de-weighting tower 300 by a pipeline.

[0029] In one possible implementation, a third condenser 530 is further included, and the third condenser 530 is arranged between the de-lightening tower 400 and the finished product tank 700; a pipeline is connected between the third outlet of the de-lightening tower 400 and the inlet end of the third condenser 530, and a pipeline is connected between the outlet end of the third condenser 530 and the inlet end of the finished product tank 700.

[0030] In one possible implementation, the first inlet of the deweighting tower 300 is set at the middle position in the height direction of the deweighting tower 300, the setting height of the second inlet of the deweighting tower 300 is lower than the setting height of the first inlet of the deweighting tower 300, and the setting height of the third inlet of the deweighting tower 300 is higher than the setting height of the first inlet of the deweighting tower 300.

[0031] In one possible implementation, the first outlet of the deweighting tower 300 is arranged at the bottom of the deweighting tower 300, and the first outlet of the deweighting tower 300 is also provided with a pipeline connected to the exhaust gas treatment system outside the device, and the second outlet of the deweighting tower 300 is arranged at the top of the deweighting tower 300.

[0032] In one possible implementation, the first inlet of the delightening tower 400 is set at the middle position in the height direction of the delightening tower 400, the setting height of the second inlet of the delightening tower 400 is lower than the setting height of the first inlet of the delightening tower 400, and the setting height of the third inlet of the delightening tower 400 is higher than the setting height of the first inlet of the delightening tower 400.

[0033] In a possible implementation, the first outlet of the de-lightness tower 400 is arranged at the top of the de-lightness tower 400 , and the second outlet and the third outlet of the de-lightness tower 400 are both arranged at the bottom of the de-lightness tower 400 .

[0034] The purity of liquid chlorine in the raw material tank 100 of the present application is 99.8%, wherein the content of hydrogen is <0.002%, the content of oxygen and argon is <0.001%, the content of nitrogen is <0.1%, the content of carbon dioxide is <0.005%, the content of carbon monoxide is <0.076%, the content of hydrocarbon is <0.003%, the content of water is <0.008%, and the content of nitrogen trichloride is <0.005%.

[0035] (1) Vaporization stage: The raw liquid chlorine is regulated by a pneumatic regulating valve at a flow rate of 50 kg / hr and enters the liquid chlorine vaporizer 200. 0°C-60°C hot water is used for vaporization and heat exchange of the liquid chlorine. The temperature of the vaporized chlorine is between 20°C and 60°C, and the pressure is between 0.5MPa and 2.0MPa.

[0036] (2) Pre-purification section: After vaporization, chlorine gas at 20℃-60℃ and 0.5MPa-2.0MPa enters the chlorine pre-purifier 800 for deep dehydration and carbon dioxide removal. Pre-purification uses high-efficiency acid-resistant 4A molecular sieves and AW series acid-resistant molecular sieves to dehydrate and remove carbon dioxide gas, and removes water and carbon dioxide in the raw chlorine gas to below 1ppm. After the molecular sieve has been used for a period of time, the adsorption efficiency decreases and desorption treatment is required. The regenerated molecular sieve is used alternately in a cycle.

[0037] (3) Distillation section: Control and ensure that the circulating hot water is 0℃-60℃, and heat the first reboiler 610 of the tower kettle of the de-weight tower 300 and the second reboiler 620 of the tower kettle of the de-light tower 400; control the circulating chilled water to -10℃-32℃, and exchange heat with the first condenser 510 and the second condenser 520 at the top of the de-weight tower 300 and the de-light tower 400. After the distillation separation begins, the pressure range of the de-weight tower 300 is controlled to be 0.5MPa-2.0MPa, the top temperature range of the de-weight tower 300 is -5℃-40℃, and the bottom temperature is -5℃-35℃; the pressure range of the de-light tower 400 is controlled to be 0.4MPa-1.8MPa, the top temperature range of the de-light tower 400 is -5℃-35℃, and the bottom temperature is -5℃-30℃. During the distillation separation process, trace amounts of water, nitrogen trichloride, metal ions and other heavy components are discharged from the bottom of the de-heavy tower 300, and the de-heavy chlorine flows out from the top gas phase of the de-heavy tower 300 into the de-light tower 400 for distillation. The top condenser of the de-light tower 400 discharges oxygen, nitrogen, argon, hydrogen, carbon monoxide, trace amounts of carbon dioxide and hydrocarbon gases out of the device. The product liquid 6N electronic grade chlorine in the bottom of the de-light tower 400 is cooled by the third condenser 530 and then enters the finished product tank 700 for storage.

[0038] It should be noted that although a chlorine purification device is introduced as an example in this application, those skilled in the art will understand that this application should not be limited thereto. In fact, the user can flexibly set various parameters according to personal preferences and / or actual application scenarios, as long as the design is reasonable.

[0039] In this way, the raw material tank is used to store untreated liquid chlorine, the liquid chlorine enters the vaporizer for heat exchange to obtain chlorine, and the chlorine enters the de-weighting tower for distillation separation. During the distillation separation process, trace amounts of water, nitrogen trichloride and metal ions in the chlorine are discharged from the de-weighting tower kettle. The de-weighted chlorine flows into the de-lighting tower after the gas phase is treated by the first condenser. The de-lighting tower and the second condenser discharge oxygen, nitrogen, argon, hydrogen, carbon monoxide, carbon dioxide and hydrocarbon gases. The generated chlorine enters the finished product tank for storage and standby. According to a chlorine purification device of the present application, a relatively simple process can be used to purify the chlorine, and no environmental pollution will be caused during the purification process.

[0040] The embodiments of the present application have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or improvements to the technology in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A chlorine purification device, characterized in that: include: Raw material tank, vaporizer, de-heavy tower, de-light tower, condenser, reboiler and finished product tank; The number of the condensers is two, namely a first condenser and a second condenser; The number of the reboilers is two, namely a first reboiler and a second reboiler; The outlet end of the raw material tank is connected to the inlet end of the vaporizer through a pipeline, and the outlet end of the vaporizer is connected to the inlet end of the deweighting tower through a pipeline; The de-weighting tower is connected to the first reboiler by a loop, the de-weighting tower is connected to the first condenser by a loop, and the outlet of the first condenser is connected to the inlet of the de-weighting tower by a pipeline; The light removal tower is connected to the second reboiler in a loop, the light removal tower is connected to the second condenser in a loop, and the outlet end of the light removal tower is connected to the finished product tank by a pipeline.

2. The chlorine purification device according to claim 1, characterized in that: The vaporizer is connected to the first inlet of the deweighting tower by a pipeline; A first outlet of the de-weighting tower is connected to an inlet of the first reboiler by a pipeline, and an outlet of the first reboiler is connected to a second inlet of the de-weighting tower by a pipeline; The second outlet of the de-weighting tower is connected to the inlet end of the first condenser by a pipeline, the first outlet of the first condenser is connected to the third inlet of the de-weighting tower by a pipeline, and the second outlet of the first condenser is connected to the first inlet of the de-weighting tower by a pipeline.

3. The chlorine purification device according to claim 2, characterized in that: A first outlet of the light-removal tower and an inlet end of the second reboiler are connected by a pipeline, and an outlet end of the second reboiler and a second inlet of the light-removal tower are connected by a pipeline; The second outlet of the light-removal tower is connected to the inlet end of the second condenser by a pipeline, and the outlet end of the second condenser is connected to the third inlet of the light-removal tower by a pipeline; The third outlet of the light removal tower is connected to the inlet end of the finished product tank by a pipeline.

4. The chlorine purification device according to any one of claims 1 to 3, characterized in that: Also included is a pre-purifier, the pre-purifier being disposed between the vaporizer and the deweighting tower; The outlet end of the vaporizer is connected to the inlet end of the pre-purifier by a pipeline, and the outlet end of the pre-purifier is connected to the inlet end of the deweighting tower by a pipeline.

5. The chlorine purification device according to any one of claims 1 to 3, characterized in that: It also includes a third condenser, which is arranged between the light removal tower and the finished product tank; The third outlet of the light removal tower is connected to the inlet end of the third condenser by a pipeline, and the outlet end of the third condenser is connected to the inlet end of the finished product tank by a pipeline.

6. The chlorine purification device according to claim 3, characterized in that: The first inlet of the deweighting tower is set at the middle position in the height direction of the deweighting tower, the second inlet of the deweighting tower is set at a height lower than the first inlet of the deweighting tower, and the third inlet of the deweighting tower is set at a height higher than the first inlet of the deweighting tower.

7. The chlorine gas purification device according to claim 6, characterized in that: The first outlet of the deweighting tower is arranged at the bottom of the deweighting tower, and the second outlet of the deweighting tower is arranged at the top of the deweighting tower.

8. The chlorine purification device according to claim 3, characterized in that: The first inlet of the de-lightness tower is arranged at the middle position in the height direction of the de-lightness tower, the second inlet of the de-lightness tower is arranged at a height lower than the first inlet of the de-lightness tower, and the third inlet of the de-lightness tower is arranged at a height higher than the first inlet of the de-lightness tower.

9. The chlorine purification device according to claim 8, characterized in that: The first outlet of the lightness removal tower is arranged at the top of the lightness removal tower, and the second outlet and the third outlet of the lightness removal tower are both arranged at the bottom of the lightness removal tower.

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