JPH03170306A - Production of nitrogen trifluoride - Google Patents
Production of nitrogen trifluorideInfo
- Publication number
- JPH03170306A JPH03170306A JP30724289A JP30724289A JPH03170306A JP H03170306 A JPH03170306 A JP H03170306A JP 30724289 A JP30724289 A JP 30724289A JP 30724289 A JP30724289 A JP 30724289A JP H03170306 A JPH03170306 A JP H03170306A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- metal fluoride
- reaction
- fluorine
- fluoride
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 title claims description 5
- 239000011737 fluorine Substances 0.000 claims abstract description 15
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910001512 metal fluoride Inorganic materials 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims abstract 3
- 239000002131 composite material Substances 0.000 claims abstract 3
- 230000008929 regeneration Effects 0.000 claims abstract 2
- 238000011069 regeneration method Methods 0.000 claims abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 abstract description 7
- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 abstract description 7
- 238000004880 explosion Methods 0.000 abstract description 5
- 238000003682 fluorination reaction Methods 0.000 abstract description 4
- KWVVTSALYXIJSS-UHFFFAOYSA-L silver(ii) fluoride Chemical compound [F-].[F-].[Ag+2] KWVVTSALYXIJSS-UHFFFAOYSA-L 0.000 abstract description 4
- 229910021571 Manganese(III) fluoride Inorganic materials 0.000 abstract description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- SRVINXWCFNHIQZ-UHFFFAOYSA-K manganese(iii) fluoride Chemical compound [F-].[F-].[F-].[Mn+3] SRVINXWCFNHIQZ-UHFFFAOYSA-K 0.000 abstract description 2
- 238000001312 dry etching Methods 0.000 abstract 1
- 229920001296 polysiloxane Polymers 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 19
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000004817 gas chromatography Methods 0.000 description 6
- 239000011698 potassium fluoride Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 235000003270 potassium fluoride Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- -1 SiJ4 Inorganic materials 0.000 description 1
- 229910008814 WSi2 Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
- C01B21/0832—Binary compounds of nitrogen with halogens
- C01B21/0835—Nitrogen trifluoride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Drying Of Semiconductors (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】 産業土勿列−肚光顆 本発明は三フッ化窒素（ＮＦｉ）の製造法に関する。[Detailed description of the invention] Industrial soil - Duguang condyle The present invention relates to a method for producing nitrogen trifluoride (NFi).
三フッ化窒素は沸点−１２９℃の無色のガスであり、Ｃ
ＶＤ装置のプラズマ洗浄用ガスとして、またシリコン、
ポリシリコン、ＳｉＪ４， ＷＳｉ２， ＭｏＳｉｚな
どのトライエッチングガス及びエキシマレーザ用ガスと
して、またＮＦ３はフッ素より適度に活性が低いフッ素
源として、また低い毒性のため、従？特に、フルオロオ
レフィンの調製におけるフッ素源としてや高エネルギー
燃料の酸化剤に用いられる工業的に重要なガスである。Nitrogen trifluoride is a colorless gas with a boiling point of -129°C.
As a plasma cleaning gas for VD equipment, silicon,
As a tri-etching gas and excimer laser gas for polysilicon, SiJ4, WSi2, MoSiz, etc., NF3 is also used as a fluorine source, which is moderately less active than fluorine, and because of its low toxicity, it has become a popular choice. In particular, it is an industrially important gas used as a fluorine source in the preparation of fluoroolefins and as an oxidizing agent in high-energy fuels.
瑳来坐技血表土■欄鳳一点
従来よりＮＦ３の製造法として種々の方法が提案されて
いる。例えば米国特許第３３０４２８号には気体窒素を
ｌ０００℃を越える温度でプラズマアーク中を通過させ
、また気体フッ素を陽極に近いポスト・アーク域に導入
することによりＮＦ３を得る方法が開示されている。Araki Zagi Blood Topsoil ■Renho One Point Various methods have been proposed for the production of NF3. For example, US Pat. No. 3,30,428 discloses a method for obtaining NF3 by passing gaseous nitrogen through a plasma arc at temperatures in excess of 1000° C. and introducing gaseous fluorine into the post-arc region near the anode.
また、特許公報昭６２−２１７２４には固体状の金属フ
ッ化物のアンモニウム錯休と元素状フッ素とを室温以上
で気固反応させてＮＦ．を製造する方法が開示されてい
る。Further, in Patent Publication No. 62-21724, NF. A method of manufacturing is disclosed.
また、特許公報昭５５−８９２６には気相状フッ素を融
解温度から実質的に４００下以下の温度までの温度に維
持された液相アンモニウム酸フッ化物と反応を行わせて
ＮＦ３を製造する方法が述べられている。Further, Patent Publication No. 55-8926 discloses a method for producing NF3 by reacting gaseous fluorine with liquid ammonium acid fluoride maintained at a temperature substantially below the melting temperature. is stated.
ジャーナル オブ アメリカン ケミカルソ→ノ゜？ア
ティ（Ｊ．八ｍ．ｃｈｅｍ，Ｓｏｃ．）８２■巻、５３
０１ページ（１９６０年）記載の論文にはアンモニア対
フッ素のモル比、約１：１から２：１を用いてアンモニ
アの直接気相フッ素化によるＮＦ３の合或について開示
している。反応条件の詳細について記載はみられないが
フッ素基準で約１０〜２５％のＮＦ３の収率を報告して
いる。Journal of American Chemical Society→No゜? Atty (J. 8m. chem, Soc.) Volume 82, 53
01 (1960) discloses the synthesis of NF3 by direct gas phase fluorination of ammonia using an ammonia to fluorine molar ratio of about 1:1 to 2:1. Although the details of the reaction conditions are not described, the yield of NF3 is reported to be about 10 to 25% based on fluorine.
米国特許第３２５４７４号には酸性フッ化アンモニウム
の溶融塩電解法について記載されている。US Pat. No. 3,254,74 describes a molten salt electrolysis process for acidic ammonium fluoride.
これらはいずれも元素状のフッ素を使用しており、第一
義的には爆発の危険性があり、従って、爆発防止のため
に種々の提案がなされているが、いずれも満足しうるも
のではなく、結果的には収率の低下を招くものである。All of these use elemental fluorine, which poses a primary risk of explosion.Therefore, various proposals have been made to prevent explosions, but none of them are satisfactory. This results in a decrease in yield.
また電解法においては酸性フッ化アンモニウムまたはフ
ッ化アンモニウムとフッ化水素を原料とするＮＨ４Ｆ
− ｝ＩＰ系やこれに更に酸性フッ化カリウムまたはフ
ッ化カリウムを原料として加えたＫＦ・ＮＨ．Ｆ −
ＩＰ系で溶融塩電解を行いＮＦ３を製造する場合、電解
槽の陽極からはＮＦ３ガスが発生し、陰極？らｌ１■ガ
スが発生する。このＮＦａとＨ２は混合すると爆発を引
き起こす。従って、その運転法に種々の工夫をする必要
がある。In addition, in the electrolytic method, NH4F using acidic ammonium fluoride or ammonium fluoride and hydrogen fluoride as raw materials is used.
- }IP system and KF/NH. which is further added with acidic potassium fluoride or potassium fluoride as raw material. F-
When NF3 is produced by molten salt electrolysis in an IP system, NF3 gas is generated from the anode of the electrolytic tank, and the cathode? l1■ Gas is generated. When NFa and H2 mix together, they cause an explosion. Therefore, it is necessary to make various improvements to the operating method.
発粧へ匪鰺
本発明の目的は、上記従来法の欠点を排除し、爆発の危
険なく、特別な装置を必要とせず、効率よ＜ＮＰ．を製
造することである。The purpose of the present invention is to eliminate the drawbacks of the above-mentioned conventional methods, to eliminate the risk of explosion, to eliminate the need for special equipment, and to improve efficiency. is to manufacture.
発朝少物雇
本発明は、アンモニアをフッ素化するにあたり、従来の
特許文献等にみられるような元素状フッ素を用いること
なく、三フッ化コバルト（ＣｏＦ３）、ニフッ化銀（Ａ
ｇＦｚ）、三フッ化マンガン（ＭｎＦ，）、及びＣｏＦ
３とＫＰの複合塩（ＫＣＯＦ４）等でフッ素化するこ
とによりＮＦ：ｌを製造する方法である。反応温度は５
０〜４５０℃の範囲が好ましい。また、アンモニアを窒
素等の不活性ガスで希釈したり、ＮＦＩで希釈してＣｏ
Ｆ＋等と反応させる等、適宜選択することができる。The present invention, when fluorinating ammonia, uses cobalt trifluoride (CoF3), silver difluoride (A
gFz), manganese trifluoride (MnF, ), and CoF
This is a method for producing NF:l by fluorination with a complex salt of 3 and KP (KCOF4). The reaction temperature is 5
A range of 0 to 450°C is preferred. In addition, ammonia can be diluted with an inert gas such as nitrogen, or diluted with NFI to produce Co.
It can be selected as appropriate, such as reacting with F+ or the like.
また本発明は反応によりフッ素化能力がなくなった金属
フッ化物を元素状フッ素で再生する際、反応により副生
したフッ化アンモニウム（ＮＨ．Ｆ）や酸性フッ化アン
モニウム（ＮＨ４Ｆ−ｎｌｌＦ）は元素状フッ素と反応
させＮＦ３を生威することが出来る。Furthermore, in the present invention, when a metal fluoride that has lost its fluorination ability due to a reaction is regenerated with elemental fluorine, ammonium fluoride (NH.F) and acidic ammonium fluoride (NH4F-nllF), which are by-produced by the reaction, are NF3 can be produced by reacting with fluorine.
従って、本発明は本反応の副生物も無駄なく利用し連続
してＮＦ３を生威することができる。Therefore, in the present invention, the by-products of this reaction can also be used without waste, and NF3 can be continuously produced.
また、本発明は元素状フッ素を利用する従来法に比べ活
性の弱い三フッ化コバルト等を使用するため反応の制御
が容易、しかも安全にＮＦ３を高収率で得ることが出来
る利点がある。Furthermore, since the present invention uses cobalt trifluoride, which has a weaker activity than the conventional method using elemental fluorine, it has the advantage that the reaction can be easily controlled and NF3 can be obtained safely in a high yield.
さらに、本発明を実施するに際し、アンモニアは一括、
分割仕込を適宜選択することが出来る。Furthermore, when carrying out the present invention, ammonia is
You can select split preparation as appropriate.
以下実施例により本発明をさらに詳細に説明する。The present invention will be explained in more detail with reference to Examples below.
実讃駆（二上
ニッケル製反応器に三フッ化コバルト（ＣＯＦ３） ヲ
５０ｋｇ仕込んだ。(50kg of cobalt trifluoride (COF3) was charged into a reactor made by Nijo Nickel.
この反応器を８０℃ （ＣＯＦ３層温度）に調節し、ア
ンモニアガスを１０ｌ／分の割合で送入した。反応ガス
を１０％水酸化カリウム水溶液が循環しているアルカリ
洗浄塔で洗浄後、ガスメーターで計量し、ガスクロマト
グラフィーによって組威を分析した。The reactor was adjusted to 80° C. (COF 3 layer temperature) and ammonia gas was fed at a rate of 10 l/min. After the reaction gas was washed in an alkaline washing tower in which a 10% aqueous potassium hydroxide solution was circulated, it was measured with a gas meter, and the composition was analyzed by gas chromatography.
その結果、平均ガス組或は次の通りであった。As a result, the average gas composition was as follows.
（ガスクロマトグラフィー面積パーセント、以下同し）
？■ ０．２％
ＮＺ ７９．３％
ＮＦ． １９．８％
その他 ０．７％
実施班二斐
実施例−１と同じ反応器で反応温度を１６０℃（ＣＯＦ
３層温度）に調節し、アンモニアと窒素の混合ガス（１
：１）を１０１！．／分の割合で送入した。(Gas chromatography area percent, hereinafter the same)? ■ 0.2% NZ 79.3% NF. 19.8% Others 0.7% The reaction temperature was set at 160℃ (COF) in the same reactor as in Example-1.
3 layer temperature), and mixed gas of ammonia and nitrogen (1
:1) 101! ．． /min.
反応ガスは１０％水酸化カリウム水溶液が循環するアル
カリ洗浄塔で洗浄後、ガスメーターで計量し、ガスクロ
マトグラフィーによって組威を分析した。The reaction gas was washed in an alkaline washing tower in which a 10% aqueous potassium hydroxide solution was circulated, then measured with a gas meter, and its composition was analyzed by gas chromatography.
その結果、平均ガス組或は次の通りであった。As a result, the average gas composition was as follows.
０２０． １％
Ｎｚ ９０．６％
ＮＦ３ Ｂ．５％
その他 ０．８％
亥１自妙二Ｊ一
実施例−１と同し反応器でＣｏＦ３の代わりにＣｏＦ．
とＫＦの複合塩（１：１）を入れ、反応器を３００℃（
ＣｏＦｒ ＫＦ層温度）６こ調節し、アンモニアガス
を１０ｌ／分の割合で送入した。反応ガスをｌＯ％水酸
化カリウム水溶液が循環しているアルカリ洗浄塔で洗浄
後、ガスメーターで計量し、ガスクロマトグラフィーに
よって平均組或を分析した。020. 1% Nz 90.6% NF3 B. 5% Others 0.8% In the same reactor as in Example-1, CoF.
and KF complex salt (1:1) and heated the reactor to 300℃ (
The temperature of the CoFr KF layer was adjusted by 6 degrees, and ammonia gas was introduced at a rate of 10 l/min. After the reaction gas was washed in an alkaline washing tower in which a 10% potassium hydroxide aqueous solution was circulated, it was measured with a gas meter, and the average composition was analyzed by gas chromatography.
０。 ０．１％
Ｎ２６５．３％
ＮＦ３ ３４．２％
その他 ０．４％
尖施握二土
実施例−Ｌ２，３それぞれ反応終了後、元素状フッ素を
５ｌ／分で送入した。反応生成ガスは１０％水酸化カリ
ウム水溶液が循環するアルカリ洗浄塔で洗浄後、ガスメ
ーターで計量し、ガスクロマトグラフィーによって組戒
を分析した。平均組戒は以下の通りであった。0. 0.1% N2 65.3% NF3 34.2% Others 0.4% After completion of each reaction, elemental fluorine was fed at a rate of 5 l/min. The reaction product gas was washed in an alkaline washing tower in which a 10% aqueous potassium hydroxide solution was circulated, then measured with a gas meter, and the composition was analyzed by gas chromatography. The average group precepts were as follows.
７
？■ ３．６％
Ｎｚ ３５．３％
Ｎｈ ５６．７％
その他 ４．４％
実施槻二五
実施例−１で使用した反応器に更にガス送入口を２ケ所
取り付け、反応器を１２０℃に調節し、３ケ所よりＮＨ
３を各々５１／分の流速で計１５ｌ／分送入した。反応
ガスを実施例ｌ〜４と同様に後処理し、ガス組或をガス
クロマトグラフィーで分析したところ平均ガス組成は次
の通りであった。7? ■ 3.6% Nz 35.3% Nh 56.7% Others 4.4% Two gas inlet ports were added to the reactor used in Example-1, and the temperature of the reactor was adjusted to 120°C. NH from 3 locations
3 were each delivered at a flow rate of 51/min for a total of 15 l/min. The reaction gas was post-treated in the same manner as in Examples 1 to 4, and the gas composition was analyzed by gas chromatography, and the average gas composition was as follows.
０２０．２％ Ｎ２ ５９．４％ ＮＦ３ ３９．３％ その他 １．１％ ８020.2% N2 59.4% NF3 39.3% Others 1.1% 8
Claims (1)
アンモニアとを５０〜４５０℃の範囲で反応させること
を特徴とする三フッ化窒素の製造法。 ２、副生するフッ化アンモニウム及び酸性フッ化アンモ
ニウムを金属フッ化物の再生反応と並行してフッ素と反
応させることを特徴とする特許請求の範囲第１項記載の
製造法。[Claims] 1. A method for producing nitrogen trifluoride, which comprises reacting a metal fluoride and/or a composite salt of a metal fluoride with ammonia at a temperature in the range of 50 to 450°C. 2. The production method according to claim 1, wherein by-produced ammonium fluoride and acidic ammonium fluoride are reacted with fluorine in parallel with the metal fluoride regeneration reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1307242A JP2800838B2 (en) | 1989-11-27 | 1989-11-27 | Nitrogen trifluoride production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1307242A JP2800838B2 (en) | 1989-11-27 | 1989-11-27 | Nitrogen trifluoride production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03170306A true JPH03170306A (en) | 1991-07-23 |
| JP2800838B2 JP2800838B2 (en) | 1998-09-21 |
Family
ID=17966749
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1307242A Expired - Lifetime JP2800838B2 (en) | 1989-11-27 | 1989-11-27 | Nitrogen trifluoride production method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2800838B2 (en) |
-
1989
- 1989-11-27 JP JP1307242A patent/JP2800838B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2800838B2 (en) | 1998-09-21 |
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