JP4182243B2 - Chlorine purification method - Google Patents
Chlorine purification method Download PDFInfo
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- JP4182243B2 JP4182243B2 JP2002178164A JP2002178164A JP4182243B2 JP 4182243 B2 JP4182243 B2 JP 4182243B2 JP 2002178164 A JP2002178164 A JP 2002178164A JP 2002178164 A JP2002178164 A JP 2002178164A JP 4182243 B2 JP4182243 B2 JP 4182243B2
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- Prior art keywords
- oxygen
- chlorine
- dichloroethane
- containing nitrogen
- crude
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Description
【０００１】
【発明の属する技術分野】
本発明は、塩素の精製方法に関するものである。更に詳しくは、窒素及び／又は酸素を含有する粗塩素から窒素及び酸素を分離する塩素の精製方法であって、窒素及び／又は酸素と塩素との分離効率に優れ、しかも設備コスト及び運転コストの観点から極めて有利な塩素の精製方法に関するものである。
【０００２】
【従来の技術】
従来、窒素及び／又は酸素を含有する粗塩素から窒素及び酸素を分離する塩素の精製方法としては、圧縮及び／又は冷却する事によって、塩素を主成分とする液体又はガスと、窒素及び／又は酸素を主成分とするガスとに分離する方法が挙げられるが、圧縮及び／又は冷却には多大なエネルギーが必要となるだけでなく、設備コストも大きく、分離効率も悪いという問題を有している。
【０００３】
【発明が解決しようとする課題】
かかる状況において、本発明が解決しようとする課題は、窒素及び／又は酸素を含有する粗塩素から窒素及び酸素を分離する塩素の精製方法であって、分離効率に優れ、しかも設備コスト及び運転コストの観点から極めて有利な塩素の精製方法を提供する点に存するものである。
【０００４】
【課題を解決するための手段】
すなわち、本発明は、窒素及び／又は酸素を含有する粗塩素から、窒素及び酸素を分離する塩素の精製方法であって、窒素及び／又は酸素を含有する粗塩素を１，２―ジクロロエタンと接触させることにより、窒素及び／又は酸素を含有する粗塩素中の塩素を１，２―ジクロロエタンに吸収させる塩素の精製に係るものである。
【０００５】
【発明の実施の形態】
本発明において用いられる窒素及び／又は酸素を含有する粗塩素としては、アルゴン、二酸化炭素、一酸化炭素や有機化合物等のガスを含むものも用いることができる。
【０００６】
本発明においては、窒素及び／又は酸素を含有する粗塩素を１，２―ジクロロエタンと接触させることにより、窒素及び／又は酸素を含有する粗塩素中の塩素を１，２―ジクロロエタンに吸収させる必要がある。このことにより、分離効率に優れ、しかも設備コスト及び運転コストの抑制を確保しうる。
【０００７】
窒素及び／又は酸素を含有する粗塩素と１，２―ジクロロエタンとの接触温度は−５０〜２００℃、好ましくは−１０〜１００℃、更に好ましくは、０〜１００℃で行われる。該温度が−５０℃よりも低い場合には、設備コストが高くなり、経済的に不利になることがあり、一方２００℃よりも高い場合には、１，２―ジクロロエタンに塩素が十分に吸収されないことがある。
【０００８】
圧力は０．１〜２ＭＰａで行われる。該圧力が０．１ＭＰａよりも低い場合には、１，２―ジクロロエタンに塩素が十分に吸収されないことがあり、一方２ＭＰａよりも高い場合には、設備コストが高くなり、経済的に不利になることがある。
【０００９】
１，２―ジクロロエタンの使用量は、窒素及び／又は酸素を含有する粗塩素中の塩素重量に対して０．１〜２００倍量、好ましくは１〜１００倍量、更に好ましくは、１〜５０倍量で実施される。１，２―ジクロロエタンの量が過小であると、塩素が十分に吸収されないことがあり、一方１，２―ジクロロエタンの量が過多であると、設備コストが高くなり、経済的に不利になることがある。
【００１０】
窒素及び／又は酸素を含有する粗塩素中の塩素を１，２―ジクロロエタンに吸収させて得られた塩素を含有する１，２―ジクロロエタンは、通常の蒸留分離方法によって、塩素と１，２―ジクロロエタンに分離後、１，２―ジクロロエタンを循環リサイクルすることができる。
【００１１】
１，２―ジクロロエタンに吸収されなかった窒素及び／又は酸素を含有するガス成分は、ガス中の１，２―ジクロロエタンを回収するために、冷却して１，２―ジクロロエタンを凝縮させて分離させた後、１，２―ジクロロエタンを循環リサイクルすることができる。冷却装置は、熱交換器等が用いられ、１段又は多段で冷却され、冷却後の温度は、―５０〜４０℃まで冷却される。冷却温度は低いほど、１，２―ジクロロエタンのロスが少なくなる。
【００１２】
本発明においては、吸収塔、冷却装置、ドラム、配管等における酸素、１，２−ジクロロエタン濃度を爆発範囲外で操作することが、装置を安全に操作する観点から好ましい。
【００１３】
本発明においては、窒素及び／又は酸素を含有する粗塩素と１，２―ジクロロエタンとを、吸収塔を用いて接触させることが接触効率を大きくする上で好ましい。吸収塔内には充填物又は棚段を用いることが、接触効率を大きくする上で更に好ましい。
【００１４】
本発明においては、１，２―ジクロロエタンの吸収塔への供給は、窒素及び／又は酸素を含有する粗塩素の供給より上部に供給することが好ましい。
【００１５】
本発明においては、塩化水素を触媒酸化及び／又は電気分解によって得られた窒素及び／又は酸素を含有する粗塩素を用いることが好ましい。中でも、塩化水素を酸化ルテニウムを含有する触媒の存在下、酸素を含有するガスで酸化することによって得られた窒素及び／又は酸素を含有する粗塩素を用いることが好ましい。
【００１６】
【実施例】
以下、本発明を実施例により説明する。なお［ ］内の数字は図１に示す機器に対応し、〈 〉内の英数字は図１に示すストリ−ムに対応する。
実施例１
冷却器［２］を備えた理論段数１０段の吸収塔［１］へ、表−１に示す組成の窒素及び酸素を含有する粗塩素〈ａ〉６０ｔ／ｈｒ、１，２―ジクロロエタン〈ｂ〉３００ｔ／ｈｒを連続的に供給し、塔頂圧力０．５ＭＰａ、塔頂温度５℃、塔底温度１８℃の条件下で接触させると、塔底部から表１に示す組成の塩素を含有する１，２―ジクロロエタン塔底液〈ｃ〉３２０ｔ／ｈｒが得られる。塔頂部の冷却器からは、表１に示す組成の窒素及び酸素を含有する塔頂ガス〈ｄ〉４０ｔ／ｈｒが得られる。
【００１７】
【表１】
【００１８】
【発明の効果】
以上説明したとおり、本発明により、窒素及び／又はは酸素を含有する粗塩素から窒素及び酸素を分離する塩素の精製方法であって、粗塩素を１，２―ジクロロエタンと接触させることにより粗塩素中の塩素を１，２―ジクロロエタンに吸収させる塩素の精製方法を提供することができた。
【図面の簡単な説明】
【図１】本発明のフローを示す図である。
【符号の説明】
１ 吸収塔
２ 冷却器
ａ 窒素及び酸素を含有する粗塩素
ｂ １，２―ジクロロエタン
ｃ 塩素を含有する１，２―ジクロロエタン塔底液
ｄ 窒素及び酸素を含有する塔頂ガス[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for purifying chlorine. More specifically, the present invention relates to a chlorine purification method for separating nitrogen and oxygen from crude chlorine containing nitrogen and / or oxygen, which is excellent in separation efficiency of nitrogen and / or oxygen and chlorine, and has equipment and operating costs. The present invention relates to a chlorine purification method that is extremely advantageous from the viewpoint.
[0002]
[Prior art]
Conventionally, as a chlorine purification method for separating nitrogen and oxygen from crude chlorine containing nitrogen and / or oxygen, a liquid or gas mainly containing chlorine and nitrogen and / or by compression and / or cooling. There is a method of separating into a gas containing oxygen as a main component, but not only compression and / or cooling requires a lot of energy, but also has a problem that equipment cost is high and separation efficiency is poor. Yes.
[0003]
[Problems to be solved by the invention]
In such a situation, the problem to be solved by the present invention is a chlorine purification method for separating nitrogen and oxygen from crude chlorine containing nitrogen and / or oxygen, which is excellent in separation efficiency, and also has equipment and operating costs. Therefore, the present invention is to provide a chlorine purification method which is extremely advantageous from the above viewpoint.
[0004]
[Means for Solving the Problems]
That is, the present invention relates to a chlorine purification method for separating nitrogen and oxygen from crude chlorine containing nitrogen and / or oxygen, wherein the crude chlorine containing nitrogen and / or oxygen is contacted with 1,2-dichloroethane. In this manner, 1,2-dichloroethane absorbs chlorine in crude chlorine containing nitrogen and / or oxygen, and relates to purification of chlorine.
[0005]
DETAILED DESCRIPTION OF THE INVENTION
As the crude chlorine containing nitrogen and / or oxygen used in the present invention, those containing gas such as argon, carbon dioxide, carbon monoxide and organic compounds can also be used.
[0006]
In the present invention, it is necessary that 1,2-dichloroethane absorbs chlorine in crude chlorine containing nitrogen and / or oxygen by contacting crude chlorine containing nitrogen and / or oxygen with 1,2-dichloroethane. There is. As a result, the separation efficiency is excellent, and it is possible to ensure the suppression of equipment cost and operation cost.
[0007]
The contact temperature between the crude chlorine containing nitrogen and / or oxygen and 1,2-dichloroethane is -50 to 200 ° C, preferably -10 to 100 ° C, and more preferably 0 to 100 ° C. When the temperature is lower than −50 ° C., the equipment cost is high, which may be economically disadvantageous. On the other hand, when the temperature is higher than 200 ° C., chlorine is sufficiently absorbed by 1,2-dichloroethane. It may not be done.
[0008]
The pressure is 0.1 to 2 MPa. If the pressure is lower than 0.1 MPa, chlorine may not be sufficiently absorbed by 1,2-dichloroethane, whereas if it is higher than 2 MPa, the equipment cost becomes high, which is economically disadvantageous. Sometimes.
[0009]
The amount of 1,2-dichloroethane used is 0.1 to 200 times, preferably 1 to 100 times, more preferably 1 to 50 times the weight of chlorine in the crude chlorine containing nitrogen and / or oxygen. Performed in double doses. If the amount of 1,2-dichloroethane is too small, chlorine may not be sufficiently absorbed. On the other hand, if the amount of 1,2-dichloroethane is excessive, the equipment cost will be high and it will be economically disadvantageous. There is.
[0010]
1,2-dichloroethane containing chlorine obtained by absorbing chlorine in crude chlorine containing nitrogen and / or oxygen into 1,2-dichloroethane is separated from chlorine by 1,2- After separation into dichloroethane, 1,2-dichloroethane can be recycled.
[0011]
The gas components containing nitrogen and / or oxygen that have not been absorbed by 1,2-dichloroethane are cooled and condensed to separate 1,2-dichloroethane in order to recover 1,2-dichloroethane in the gas. After that, 1,2-dichloroethane can be recycled. As the cooling device, a heat exchanger or the like is used, and it is cooled in one or more stages, and the temperature after cooling is cooled to −50 to 40 ° C. The lower the cooling temperature, the less 1,2-dichloroethane loss.
[0012]
In the present invention, it is preferable to operate oxygen and 1,2-dichloroethane concentrations in the absorption tower, cooling device, drum, piping, etc. outside the explosion range from the viewpoint of operating the device safely.
[0013]
In the present invention, it is preferable to bring crude chlorine containing nitrogen and / or oxygen into contact with 1,2-dichloroethane using an absorption tower in order to increase the contact efficiency. In order to increase the contact efficiency, it is more preferable to use a packing or a shelf in the absorption tower.
[0014]
In the present invention, the supply of 1,2-dichloroethane to the absorption tower is preferably performed above the supply of crude chlorine containing nitrogen and / or oxygen.
[0015]
In the present invention, it is preferable to use crude chlorine containing nitrogen and / or oxygen obtained by catalytic oxidation and / or electrolysis of hydrogen chloride. Among them, it is preferable to use nitrogen and / or crude chlorine containing oxygen obtained by oxidizing hydrogen chloride with a gas containing oxygen in the presence of a catalyst containing ruthenium oxide.
[0016]
【Example】
Hereinafter, the present invention will be described with reference to examples. The numbers in [] correspond to the device shown in FIG. 1, and the alphanumeric characters in <> correspond to the stream shown in FIG.
Example 1
Crude chlorine <a> 60 t / hr, 1,2-dichloroethane <b> containing nitrogen and oxygen having the composition shown in Table 1 to an absorption tower [1] having 10 theoretical plates equipped with a cooler [2] When 300 t / hr is continuously supplied and contacted under the conditions of a tower top pressure of 0.5 MPa, a tower top temperature of 5 ° C., and a tower bottom temperature of 18 ° C., 1 containing chlorine having the composition shown in Table 1 from the tower bottom. , 2-dichloroethane tower bottom liquid <c> 320 t / hr. A tower top gas <d> 40 t / hr containing nitrogen and oxygen having the composition shown in Table 1 is obtained from the tower top cooler.
[0017]
[Table 1]
[0018]
【The invention's effect】
As described above, according to the present invention, a chlorine purification method for separating nitrogen and oxygen from crude chlorine containing nitrogen and / or oxygen, wherein the crude chlorine is brought into contact with 1,2-dichloroethane. It was possible to provide a method for purifying chlorine by allowing 1,2-dichloroethane to absorb the chlorine contained therein.
[Brief description of the drawings]
FIG. 1 is a diagram showing a flow of the present invention.
[Explanation of symbols]
DESCRIPTION OF
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002178164A JP4182243B2 (en) | 2001-06-28 | 2002-06-19 | Chlorine purification method |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001196168 | 2001-06-28 | ||
| JP2001-196168 | 2001-06-28 | ||
| JP2002178164A JP4182243B2 (en) | 2001-06-28 | 2002-06-19 | Chlorine purification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003081612A JP2003081612A (en) | 2003-03-19 |
| JP4182243B2 true JP4182243B2 (en) | 2008-11-19 |
Family
ID=26617730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002178164A Expired - Fee Related JP4182243B2 (en) | 2001-06-28 | 2002-06-19 | Chlorine purification method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4182243B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2881732B1 (en) * | 2005-02-08 | 2007-11-02 | Solvay | PROCESS FOR THE PURIFICATION OF HYDROGEN CHLORIDE |
-
2002
- 2002-06-19 JP JP2002178164A patent/JP4182243B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2003081612A (en) | 2003-03-19 |
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