JP2521133B2 - Purification method of acetylene gas - Google Patents
Purification method of acetylene gasInfo
- Publication number
- JP2521133B2 JP2521133B2 JP63196036A JP19603688A JP2521133B2 JP 2521133 B2 JP2521133 B2 JP 2521133B2 JP 63196036 A JP63196036 A JP 63196036A JP 19603688 A JP19603688 A JP 19603688A JP 2521133 B2 JP2521133 B2 JP 2521133B2
- Authority
- JP
- Japan
- Prior art keywords
- acetylene gas
- amount
- gas
- hydrogen phosphide
- activated carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、アセチレンガスの精製方法に関するもので
あり、更に詳しくは、アセチレンガス中に含まれるリン
化水素を、リン化水素量の20〜30倍量に全ガス量の1.5
×10-5倍量を加えた酸素の存在下において、賦活された
活性炭によりアセチレンガス中のリン化水素にを処理す
ることを特徴とするアセチレンガスの精製方法に関する
ものである。TECHNICAL FIELD The present invention relates to a method for purifying acetylene gas, and more specifically, the hydrogen phosphide contained in acetylene gas is contained in an amount of 20 to 20% of the hydrogen phosphide. 1.5 times the total amount of gas in 30 times
The present invention relates to a method for purifying acetylene gas, which comprises treating hydrogen phosphide in acetylene gas with activated carbon in the presence of oxygen added in an amount of × 10 -5 times.
カーバイト法により製造された粗アセチレンガス中に
は、メタン、エタン、エチレン、ベンゼン、イオウ化合
物、リン化合物、その他多種類の不純物が存在すること
が知られている。It is known that crude acetylene gas produced by the carbide method contains methane, ethane, ethylene, benzene, sulfur compounds, phosphorus compounds and various other impurities.
特にリン化水素は、人体に対して有害であると同時
に、溶接用として用いられた場合、溶接面での強度を劣
化させることが知られている。In particular, hydrogen phosphide is known to be harmful to the human body and, at the same time, to deteriorate the strength at the welding surface when used for welding.
従来、上記問題を解決するため、粗アセチレンガス
は、固体清浄剤、もしくは次亜鉛酸水溶液を用いてリン
化水素を除去した後、アセチレン容器へ充填されてお
り、溶接用として用いられるアセチレンガス中のリン化
水素の濃度は、JIS K 1902に記載されている様に、硝酸
銀水溶液（10重量パーセント）で着色しない程度で十分
であった。Conventionally, in order to solve the above-mentioned problems, crude acetylene gas has been filled in an acetylene container after removing hydrogen phosphide using a solid detergent or an aqueous solution of hypozinc acid, and the acetylene gas used for welding is used. As described in JIS K 1902, the concentration of hydrogen phosphide of was sufficient so that it was not colored with an aqueous silver nitrate solution (10 weight percent).
しかし、近年アセチレンガスはその高い反応性によ
り、ダイヤモンド薄膜、アモルファスシリコン太陽電
池、ポリアセチレン、チタンカーバイトなどの原料とし
て注目をされてきており、アセチレンガス中の微量の不
純物の存在が問題視されてきている。However, due to its high reactivity, acetylene gas has recently been attracting attention as a raw material for diamond thin films, amorphous silicon solar cells, polyacetylene, titanium carbide, etc., and the presence of trace impurities in acetylene gas has been a problem. ing.
特に不純物としてのリン化水素は、反応性が高いた
め、低濃度領域まで除去する必要がある。In particular, hydrogen phosphide as an impurity is highly reactive, so it is necessary to remove even low-concentration regions.
しかし、上記固体清浄剤では低濃度領域までリン化水
素を除去するためには大量の固体清浄剤が必要となり、
経済的及び設備的に問題があった。However, in the above solid detergent, a large amount of solid detergent is required to remove hydrogen phosphide to a low concentration region,
There were financial and facility problems.
又、次亜鉛酸水溶液で処理した場合は、製品ガス中に
は常に10ppb程度のリン化水素が存在し、1ppb以下の濃
度とするのは困難であった。Further, when treated with an aqueous solution of hypozinc acid, hydrogen phosphide of about 10 ppb was always present in the product gas, and it was difficult to make the concentration below 1 ppb.
本発明は、アセチレンガス中に存在するリン化水素を
酸素の存在下において、活性炭処理することにより、ア
セチレン中のリン化水素を低濃度領域まで容易に精製処
理することを特徴とするアセチレンガス精製方法に関す
るものである。The present invention, acetylene gas purification, characterized in that hydrogen phosphide present in acetylene gas is treated with activated carbon in the presence of oxygen to easily purify hydrogen phosphide in acetylene to a low concentration region. It is about the method.
以下、本発明の内容について詳細な説明を行う。 The details of the present invention will be described below.
本発明で使用する活性炭は、特に規定するものではな
いが、圧力損失など操作上の理由で粒状活性炭が好まし
く用いられる。又、その使用に当たっては賦活処理を施
しておくことが必要である。賦活処理は、真空中もしく
はヘリウム、窒素などの不活性ガス雰囲気下で、250〜4
00℃、好ましくは300〜350℃で３時間以上加熱処理を施
すのがよい。加熱処理温度が上記温度より低い場合は、
十分な吸着能力を得ることができず、又、上記温度より
高い場合は吸着剤自体の劣化が生じ、十分な吸着能力を
得ることができない。The activated carbon used in the present invention is not particularly specified, but granular activated carbon is preferably used for operational reasons such as pressure loss. In addition, it is necessary to carry out activation treatment before use. The activation treatment is carried out in a vacuum or in an atmosphere of an inert gas such as helium or nitrogen at 250 to 4
It is preferable to perform heat treatment at 00 ° C, preferably 300 to 350 ° C for 3 hours or more. If the heat treatment temperature is lower than the above temperature,
Sufficient adsorption capacity cannot be obtained, and if the temperature is higher than the above temperature, the adsorbent itself deteriorates and sufficient adsorption capacity cannot be obtained.
この賦活された活性炭を用い、酸素量がリン化水素量
の20〜30倍量に全ガス量の1.5×10-5倍量を加えた量に
調整された粗アセチレンガスを処理することにより、効
率よくリン化水素を精製処理することができる。酸素量
の調整は特に規定するものではないが、予め粗アセチレ
ンガス中の酸素量を測定し、活性炭処理前に必要酸素量
を粗アセチレンガスと混合し、精製処理するのが良い。
被処理ガス中の酸素量が上記に示した量以下の場合、全
く吸着が起こらないか、もしくは吸着能力は著しく低下
し好ましくない。Using this activated carbon activated, by treating the crude acetylene gas adjusted to have an oxygen amount of 20 to 30 times the hydrogen phosphide amount plus 1.5 x 10 -5 times the total gas amount, The hydrogen phosphide can be efficiently purified. The adjustment of the oxygen amount is not particularly specified, but it is preferable to measure the oxygen amount in the crude acetylene gas in advance, mix the required oxygen amount with the crude acetylene gas before the activated carbon treatment, and perform the purification treatment.
When the amount of oxygen in the gas to be treated is not more than the amount shown above, no adsorption occurs or the adsorption capacity is significantly reduced, which is not preferable.
また、上記に示した酸素量以上の場合、精製処理能力
の向上が認められないと同時に爆発の危険性が生じ、安
全上好ましくない。On the other hand, when the amount of oxygen is more than that shown above, no improvement in the refining treatment capacity is observed and, at the same time, there is a risk of explosion, which is not preferable for safety.
この活性炭による精製処理は通常の物理吸着ではな
く、酸素−リン化水素−活性炭間での化学反応を伴う化
学吸着と考えられるが、詳細は不明である。It is considered that the purification treatment with activated carbon is not normal physical adsorption but chemical adsorption involving a chemical reaction between oxygen-hydrogen phosphide-activated carbon, but details are unknown.
精製処理温度は低い程処理能力は増加するが、温度が
低すぎるとアセチレンの液化が生じ、安全上及び操作上
好ましくなく、また、精製処理温度が高すぎると、リン
化水素の精製処理能力が低下し好ましくなく、精製処理
温度は−15〜45℃、好ましくは−10〜30℃で処理するの
がよい。The lower the refining treatment temperature, the higher the treatment capacity, but if the temperature is too low, acetylene is liquefied, which is unfavorable for safety and operation.Moreover, if the refining treatment temperature is too high, the refining treatment capacity for hydrogen phosphide is too high. The treatment temperature is -15 to 45 ° C, preferably -10 to 30 ° C.
精製処理圧力は、安全上及び操作上の理由から絶対圧
力26kg/cm2以下で行うのがよい。For safety and operation reasons, it is recommended that the purification treatment pressure be performed at an absolute pressure of 26 kg / cm 2 or less.
実施例−１ 粒状活性炭80g（北越炭素製Ｙ−６）を直径1inch、長
さ30cmの吸着管に封入し、N2ガスを毎分0.5Nで流しな
がら、300℃で４時間賦活処理を施した。この賦活され
た活性炭を用い、リン化水素量１×10-3ml/、酸素量
１×10-2ml/の粗アセチレンガスを毎分1Nと、粗ア
セチレンガス中の酸素量が、リン化水素量の20倍量に全
ガス量の1.5×10-5倍量を加えた量の3.5×102ml/とな
る様に酸素ガスを毎分2.5×10-2mlの割合で活性炭入口
で混合した後、絶対圧力1kg/cm2、精製処理温度18℃で
処理した。Example-1 80 g of granular activated carbon (Y-6 manufactured by Hokuetsu Carbon Co., Ltd.) was sealed in an adsorption tube having a diameter of 1 inch and a length of 30 cm, and activated at 300 ° C. for 4 hours while flowing N 2 gas at 0.5 N per minute. did. Using this activated charcoal, 1N of crude acetylene gas with hydrogen phosphide amount of 1 × 10 -3 ml / and oxygen amount of 1 × 10 -2 ml / was added, and the amount of oxygen in the crude acetylene gas was phosphatized. Oxygen gas at the rate of 2.5 × 10 -2 ml / min at the activated carbon inlet to obtain 3.5 × 10 2 ml / of 20 times the amount of hydrogen plus 1.5 × 10 -5 times the total amount of gas. After mixing, the mixture was treated at an absolute pressure of 1 kg / cm 2 and a purification treatment temperature of 18 ° C.
粗アセチレンガスを1500処理後の吸着管出口のリン
化水素濃度はガスクロマトグラフ検出器FPDで測定した
結果、1ppb以下であった。The hydrogen phosphide concentration at the outlet of the adsorption tube after 1500 treatment of crude acetylene gas was 1 ppb or less as a result of measurement with a gas chromatograph detector FPD.
実施例−２ 粒状活性炭80g（北越炭素製Ｙ−６）を直径1inch、長
さ30cmの吸着管に封入し、N2ガスを毎分1Nで流しなが
ら330℃で４時間賦活処理を施した。Example-2 80 g of granular activated carbon (Y-6 manufactured by Hokuetsu Carbon Co., Ltd.) was enclosed in an adsorption tube having a diameter of 1 inch and a length of 30 cm, and activated at 330 ° C. for 4 hours while flowing N 2 gas at 1 N per minute.
この賦活された活性炭を用い、リン化水素量１×10-2
ml/、酸素量2.5×10-2ml/の粗アセチレンガス毎分1
Nと、粗アセチレンガス中の酸素量が、リン化水素量
の30倍量に全ガス量の1.5×10-5倍量を加えた量の31.5
×10-2ml/となる様に酸素ガスを毎分29×10-2mlの割
合で活性炭入口で混合した後、絶対圧力3kg/cm2、精製
処理温度30℃で処理した。Using this activated activated carbon, hydrogen phosphide amount 1 × 10 -2
ml /, oxygen amount 2.5 × 10 -2 ml / crude acetylene gas 1 / min
N and the amount of oxygen in the crude acetylene gas is 31.5 times the amount of 30 times the amount of hydrogen phosphide plus 1.5 × 10 -5 times the total amount of gas.
After mixing with activated carbon inlet at a rate of × 10 -2 ml / per minute and oxygen gas as made 29 × 10 -2 ml, absolute pressure 3 kg / cm 2, and treated with purification treatment temperature 30 ° C..
粗アセチレンガス1500処理後の吸着管出口のリン化
水素濃度はガスクロマトグラフ検出器FPDで測定した結
果、1ppb以下であった。The hydrogen phosphide concentration at the outlet of the adsorption tube after the treatment with crude acetylene gas 1500 was 1 ppb or less as a result of measurement with a gas chromatograph detector FPD.
比較例−１ 実施例−１同様の条件で賦活された活性炭を用い、リ
ン化水素量１×10-3ml/、酸素量１×10-2ml/の粗ア
セチレンガスを、毎分1N、絶対圧力1kg/cm2、精製処
理温度18℃で処理した。粗アセチレンガスを20処理後
の吸着管出口でのリン化水素濃度はガスクロマトグラフ
検出器FPDで測定した結果で0.5ppmであった。Comparative Example-1 Using activated carbon activated under the same conditions as in Example-1, crude acetylene gas having a hydrogen phosphide amount of 1 × 10 −3 ml / and an oxygen amount of 1 × 10 −2 ml / was added at 1 N / min. It was processed at an absolute pressure of 1 kg / cm 2 and a purification processing temperature of 18 ° C. The hydrogen phosphide concentration at the outlet of the adsorption tube after 20 treatments of crude acetylene gas was 0.5 ppm as a result of measurement by a gas chromatograph detector FPD.
以上述べた様に、本発明によれば、アセチレンガス中
のリン化水素を酸素の存在下で活性炭処理を行うことに
より、リン化水素を1ppb以下の低濃度まで容易に精製処
理することができ、工業的に有用な発明である。As described above, according to the present invention, hydrogen phosphide in acetylene gas is subjected to activated carbon treatment in the presence of oxygen, whereby hydrogen phosphide can be easily purified to a low concentration of 1 ppb or less. It is an industrially useful invention.
Claims (3)
除去するに当り、該アセチレンガスに酸素を添加して活
性炭処理することを特徴とするアセチレンガスの精製方
法。1. A method for purifying acetylene gas, which comprises removing oxygen from hydrogen phosphide contained in acetylene gas by adding oxygen to the acetylene gas and treating with activated carbon.
を特徴とする請求項１記載のアセチレンガスの精製方
法。2. The method for purifying acetylene gas according to claim 1, wherein the activated carbon has been activated.
を、該リン化水素量の20〜30倍量に全ガス量の1.5×10
-5倍量を加えた量の酸素の存在下で活性炭処理を行うこ
とを特徴とするアセチレンガスの精製方法。3. The amount of hydrogen phosphide contained in acetylene gas is 20 to 30 times the amount of hydrogen phosphide and 1.5 × 10 5 of the total amount of gas.
A method for purifying acetylene gas, which comprises performing activated carbon treatment in the presence of an amount of oxygen added by 5 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63196036A JP2521133B2 (en) | 1988-08-08 | 1988-08-08 | Purification method of acetylene gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63196036A JP2521133B2 (en) | 1988-08-08 | 1988-08-08 | Purification method of acetylene gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0245428A JPH0245428A (en) | 1990-02-15 |
| JP2521133B2 true JP2521133B2 (en) | 1996-07-31 |
Family
ID=16351136
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63196036A Expired - Lifetime JP2521133B2 (en) | 1988-08-08 | 1988-08-08 | Purification method of acetylene gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2521133B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19626484C2 (en) * | 1996-07-02 | 2000-05-04 | Linde Ag Werksgruppe Tech Gase | Process for removing hydrogen sulfide, ammonia, phosphorus and arsenic from acetylene |
-
1988
- 1988-08-08 JP JP63196036A patent/JP2521133B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0245428A (en) | 1990-02-15 |
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