JP2000169141A - Production of ammonium hexafluoroaluminate - Google Patents
Production of ammonium hexafluoroaluminateInfo
- Publication number
- JP2000169141A JP2000169141A JP10351001A JP35100198A JP2000169141A JP 2000169141 A JP2000169141 A JP 2000169141A JP 10351001 A JP10351001 A JP 10351001A JP 35100198 A JP35100198 A JP 35100198A JP 2000169141 A JP2000169141 A JP 2000169141A
- Authority
- JP
- Japan
- Prior art keywords
- ammonium
- alf
- reaction
- hexafluoroaluminum
- ammonia
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title abstract 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 18
- 238000000034 method Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 12
- -1 ammonium tetrafluoroaluminate Chemical compound 0.000 abstract description 5
- 229910020027 (NH4)3AlF6 Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 21
- 239000002994 raw material Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 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 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 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 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 208000035404 Autolysis Diseases 0.000 description 1
- 206010057248 Cell death Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BJAHYFBKECKXCD-UHFFFAOYSA-N O(F)F.N Chemical compound O(F)F.N BJAHYFBKECKXCD-UHFFFAOYSA-N 0.000 description 1
- FOJJCOHOLNJIHE-UHFFFAOYSA-N aluminum;azane Chemical compound N.[Al+3] FOJJCOHOLNJIHE-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- JUINSXZKUKVTMD-UHFFFAOYSA-N hydrogen azide Chemical compound N=[N+]=[N-] JUINSXZKUKVTMD-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 1
- 229910000127 oxygen difluoride Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000028043 self proteolysis Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体製造装置等
のクリーニングガスとして有用な三フッ化窒素の製造原
料として用いられるヘキサフルオロアルミニウムアンモ
ニウムの製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing hexafluoroaluminum ammonium used as a raw material for producing nitrogen trifluoride, which is useful as a cleaning gas for semiconductor production equipment and the like.
【０００２】[0002]
【従来技術】三フッ化窒素［ＮＦ3］は、通常無色のガ
スで、沸点約−１２９℃、融点約−２０８℃の半導体製
造装置等のクリーニングガスとして使用されている。こ
のＮＦ3の製造方法としては、種々提案されており、例
えば、米国特許第３３０４２４８号には、気体窒素を、
１０００℃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出来る限り近いポスト・
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。2. Description of the Related Art Nitrogen trifluoride [NF 3 ] is a colorless gas which is used as a cleaning gas for semiconductor manufacturing equipment having a boiling point of about -129 ° C. and a melting point of about -208 ° C. Various methods for producing NF 3 have been proposed. For example, US Pat.
Pass through a plasma arc at a temperature exceeding 1000 ° C., and post gas fluorine as close as possible to the anode.
A method for obtaining NF 3 by introducing it into the arc region is disclosed.
【０００３】このほか、アジ化水素酸ガスと二フッ化酸
素との反応、アンモニアの直接フッ素化等の気相反応が
知られている。また、アンモニウム・酸フッ化物の溶融
塩電解も知られている。しかし、これらの方法は、いず
れも反応が気相であるために、反応の制御が困難であっ
たり、可燃性または爆発性の水素を含有する雰囲気の発
生を防止することが必要である。[0003] In addition, gas phase reactions such as a reaction between hydrazoic acid gas and oxygen difluoride and a direct fluorination of ammonia are known. Also, molten salt electrolysis of ammonium / oxyfluoride is known. However, in any of these methods, since the reaction is in a gas phase, it is necessary to prevent the reaction from being difficult to control or to prevent the generation of an atmosphere containing flammable or explosive hydrogen.
【０００４】さらに、特公昭５５−８９２６号公報に
は、アンモニア酸フッ化物を溶融状態にて気体フッ素と
反応する方法が開示されている。しかし、この方法は、
気液反応であるために、反応の制御が必ずしも容易では
なく、装置の腐食が著しく、また、ＮＦ3の収率も低く
工業的には、十分な方法ではない。Further, Japanese Patent Publication No. 55-8926 discloses a method of reacting ammonium oxyfluoride with gaseous fluorine in a molten state. However, this method
Because of the gas-liquid reaction, the control of the reaction is not always easy, the corrosion of the apparatus is remarkable, and the yield of NF 3 is low, which is not an industrially sufficient method.
【０００５】かかる不都合を解決するものとして、特開
昭６０−７１５０３号公報には、固体状の金属フッ化
物、例えばヘキサフルオロアルミニウムアンモニウム
［（ＮＨ 4）3ＡｌＦ6］と元素状フッ素とを室温以上で
反応させる方法が開示されている。[0005] To solve such inconvenience, Japanese Patent Application Laid-Open
JP-A-60-71503 discloses solid metal fluoride.
Object, such as ammonium hexafluoroaluminum
[(NH Four)ThreeAlF6] And elemental fluorine at room temperature or higher
A method of reacting is disclosed.
【０００６】この（ＮＨ4）3ＡｌＦ6の工業的製造法に
ついては、一般的ではないが、少量を製造する方法とし
ては、新生の水酸化アルミニウムをフッ化アンモニウム
水溶液に入れて煮沸する、或いはフッ化アンモニウム水
溶液と水酸化アルミニウムをフッ酸溶解したものとを反
応させて得る方法が知られている。[0006] Although industrial production of (NH 4 ) 3 AlF 6 is not common, as a method for producing a small amount, fresh aluminum hydroxide is put into an aqueous ammonium fluoride solution and boiled. A method is known in which an aqueous solution of ammonium fluoride is reacted with a solution of aluminum hydroxide dissolved in hydrofluoric acid.
【０００７】しかし、このようにして得られる（Ｎ
Ｈ4）3ＡｌＦ6は、粒径が小さく、また、嵩密度が小さ
いため、ＮＦ3を製造するための原料としては必ずしも
十分なものではない。具体的には、粒径が小さいと元素
状フッ素との反応が急激に進行し、反応系温度の制御が
容易ではなくなり、反応温度が大幅に上昇することとな
るため、（ＮＨ4）3ＡｌＦ6が自己分解を起こし、ＮＦ3
の収率が低下することである。また、嵩密度が小さいと
装置容積効率が悪くなるなどの問題がある。その他、粉
塵の発生等が生じるなどの取り扱い上の問題がある。However, the thus obtained (N
Since H 4 ) 3 AlF 6 has a small particle size and a small bulk density, it is not always sufficient as a raw material for producing NF 3 . Specifically, if the particle size is small, the reaction with elemental fluorine proceeds rapidly, and it becomes difficult to control the reaction system temperature, and the reaction temperature rises significantly, so that (NH 4 ) 3 AlF 6 undergoes autolysis and NF 3
Is to decrease the yield. Further, when the bulk density is small, there is a problem that the volumetric efficiency of the apparatus is deteriorated. In addition, there is a problem in handling such as generation of dust.
【０００８】そのため前記不都合を解決するものとし
て、特開平６−３４５４２１号公報には、テトラフルオ
ロアルミニウムアンモニウム［ＮＨ4ＡｌＦ4］のフッ酸
溶液スラリーとアンモニアとの反応において、かかる目
的を達成している。しかし、原料のＮＨ4ＡｌＦ4は、一
般には製造されてなく、フッ酸に水酸化アルミニウムを
溶解し、アンモニアで中和することで得られるが、その
ための製造工程を必要とする。As a solution to the above disadvantage, Japanese Unexamined Patent Publication No. Hei 6-345421 discloses a technique for achieving the above object in a reaction between a hydrofluoric acid solution slurry of ammonium tetrafluoroaluminum [NH 4 AlF 4 ] and ammonia. I have. However, NH 4 AlF 4 as a raw material is not generally produced, but can be obtained by dissolving aluminum hydroxide in hydrofluoric acid and neutralizing it with ammonia. However, a production process for this is required.
【０００９】従って、ＮＦ3の製造において、（ＮＨ4）
3ＡｌＦ6と元素状フッ素を反応させた場合、反応残滓と
して得られるＮＨ4ＡｌＦ4を使用するリサイクル工程を
とることが好ましい。Accordingly, in the production of NF 3 , (NH 4 )
When 3 AlF 6 is reacted with elemental fluorine, it is preferable to take a recycling step using NH 4 AlF 4 obtained as a reaction residue.
【００１０】しかし、反応残滓として得られるＮＨ4Ａ
ｌＦ4には、未反応の（ＮＨ4）3ＡｌＦ6が残存する。こ
の未反応の（ＮＨ4）3ＡｌＦ6の含有量は、ＮＦ3の製造
条件により異なる。すなわち、ＮＦ3の生産性及び原料
の元素状フッ素の効率を高めるためには、未反応の（Ｎ
Ｈ4）3ＡｌＦ6の含有量は高くなる。この未反応の（Ｎ
Ｈ4）3ＡｌＦ6を含有するＮＨ4ＡｌＦ4を原料にして特
開平６−３４５４２１号公報記載の方法で製造した場
合、晶出する（ＮＨ4）3ＡｌＦ6の粒径及び嵩密度は小
さくなり、ＮＦ3を製造する原料としては必ずしも十分
なものではない。However, NH 4 A obtained as a reaction residue
Unreacted (NH 4 ) 3 AlF 6 remains in IF 4 . The content of the unreacted (NH 4 ) 3 AlF 6 varies depending on the NF 3 production conditions. That is, in order to increase the productivity of NF 3 and the efficiency of elemental fluorine as a raw material, unreacted (N
The content of H 4 ) 3 AlF 6 increases. This unreacted (N
When NH 4 AlF 4 containing H 4 ) 3 AlF 6 is used as a raw material and produced by the method described in JP-A-6-345421, the particle size and bulk density of crystallized (NH 4 ) 3 AlF 6 are small. Therefore, it is not always sufficient as a raw material for producing NF 3 .
【００１１】[0011]
【問題点を解決するための具体的手段】本発明者らは、
前記問題点を解決するため鋭意検討した結果、（Ｎ
Ｈ4）3ＡｌＦ6を含有するＮＨ4ＡｌＦ4のフッ酸溶液ス
ラリーとアンモニアとの反応において、種晶を添加して
反応させることによりかかる目的を達成することができ
ることを見い出し本発明に到達した。[Specific means for solving the problems]
As a result of intensive studies to solve the above problems, (N
In the reaction between NH 4 AlF 4 -containing hydrofluoric acid solution slurry containing H 4 ) 3 AlF 6 and ammonia, it has been found that such an object can be achieved by adding a seed crystal and reacting the same, and arrived at the present invention. .
【００１２】すなわち本発明は、ヘキサフルオロアルミ
ニウムアンモニウム［（ＮＨ4）3ＡｌＦ6］を含有する
テトラフルオロアルミニウムアンモニウム［ＮＨ4Ａｌ
Ｆ4］のフッ酸溶液スラリーとアンモニアとを反応させ
る際に、種晶をヘキサフルオロアルミニウムアンモニウ
ム［（ＮＨ4）3ＡｌＦ6］を含有するテトラフルオロア
ルミニウムアンモニウム［ＮＨ4ＡｌＦ4］に対して５〜
３０重量％添加することを特徴とするヘキサフルオロア
ルミニウムアンモニウム［（ＮＨ4）3ＡｌＦ6］の製造
方法であり、そのテトラフルオロアルミニウムアンモニ
ウム［ＮＨ4ＡｌＦ4］中のヘキサフルオロアルミニウム
アンモニウム［（ＮＨ4）3ＡｌＦ6］の含有量が５〜５
０重量％の範囲であるヘキサフルオロアルミニウムアン
モニウム［（ＮＨ4）3ＡｌＦ6］の製造方法を提供する
ものである。That is, the present invention relates to a tetrafluoroaluminum ammonium [NH 4 Al] containing hexafluoroaluminum ammonium [(NH 4 ) 3 AlF 6 ].
When a hydrofluoric acid solution slurry of F 4 ] is reacted with ammonia, a seed crystal is formed with respect to tetrafluoroaluminum ammonium [NH 4 AlF 4 ] containing hexafluoroaluminum ammonium [(NH 4 ) 3 AlF 6 ]. ~
Hexafluoro ammonium aluminum, characterized by adding 30 wt% [(NH 4) 3 AlF 6] a method for producing hexafluoro aluminum ammonium [(NH 4 in the tetrafluoro aluminum ammonium [NH 4 AlF 4] ) 3 AlF 6 ] is 5 to 5
It is intended to provide a method for producing hexafluoroaluminum ammonium [(NH 4 ) 3 AlF 6 ] in the range of 0% by weight.
【００１３】以下、本発明の方法について詳細に説明す
る。本発明において、使用する原料は、（ＮＨ4）3Ａｌ
Ｆ6を含有するＮＨ4ＡｌＦ 4、フッ酸、アンモニア、種
晶である。先ず種晶と水を仕込んだ後、（ＮＨ4）3Ａｌ
Ｆ6を含有するＮＨ4ＡｌＦ4のフッ酸溶液スラリーとア
ンモニアとを反応ｐＨが中性になるように同時に添加
し、反応させる。反応終了後の（ＮＨ4）3ＡｌＦ6のス
ラリーは、固液分離、洗浄し１５０℃程度で乾燥させ
る。その結果、平均粒子径２００μｍ以上、嵩密度１．
０ｇ／ｃｍ3以上の（ＮＨ4）3ＡｌＦ6が得られる。Hereinafter, the method of the present invention will be described in detail.
You. In the present invention, the raw material used is (NHFour)ThreeAl
F6Containing NHFourAlF Four, Hydrofluoric acid, ammonia, seed
It is a crystal. After the seed crystal and water are charged, (NHFour)ThreeAl
F6Containing NHFourAlFFourHydrofluoric acid solution slurry and
Simultaneously with ammonia to make the reaction pH neutral
And react. (NHFour)ThreeAlF6No
The rally is solid-liquid separated, washed and dried at about 150 ° C.
You. As a result, the average particle diameter was 200 μm or more, and the bulk density was 1.
0 g / cmThreeThe above (NHFour)ThreeAlF6Is obtained.
【００１４】原料のＮＨ4ＡｌＦ4に含有する（ＮＨ4）3
ＡｌＦ6量は、５〜５０重量％の範囲が好ましい。かか
る範囲未満では種晶の効果が見られない。またこの範囲
を超えると粒子径、嵩密度ともに小さいものとなる。従
って、（ＮＨ4）3ＡｌＦ6含有量がこの範囲を超える場
合、２００〜３５０℃で加熱分解させてこの範囲内に調
整したものを使用してもよい。(NH 4 ) 3 contained in the raw material NH 4 AlF 4
The amount of AlF 6 is preferably in the range of 5 to 50% by weight. Below this range, the effect of the seed crystal is not observed. If it exceeds this range, both the particle diameter and the bulk density will be small. Therefore, when the content of (NH 4 ) 3 AlF 6 exceeds this range, it is possible to use one that is decomposed by heating at 200 to 350 ° C. and adjusted to fall within this range.
【００１５】また、原料の（ＮＨ4）3ＡｌＦ6を含有す
るＮＨ4ＡｌＦ4の粒子径は、特に限定するものではない
が、平均粒子径２０〜１００μｍのものを使用すること
によりＮＨ4ＡｌＦ4から（ＮＨ4）3ＡｌＦ6への反応が
進みやすく、（ＮＨ4）3ＡｌＦ6の純度（含有率）が高
くなる。[0015] The particle diameter of NH 4 AlF 4, containing a raw material of a (NH 4) 3 AlF 6 is not particularly limited, NH 4 AlF By using the mean particle diameter of 20~100μm The reaction from 4 to (NH 4 ) 3 AlF 6 easily proceeds, and the purity (content) of (NH 4 ) 3 AlF 6 increases.
【００１６】種晶の添加量は、原料の（ＮＨ4）3ＡｌＦ
6を含有するＮＨ4ＡｌＦ4の重量に対して、５〜３０重
量％の範囲が好ましい。かかる範囲未満では効果が少な
く、またこの範囲を超えても平均粒径や嵩密度などの粉
体物性に顕著な効果は見られない。また、種晶は、純度
の面から（ＮＨ4）3ＡｌＦ6が好ましい。The amount of the seed crystal added is (NH 4 ) 3 AlF
The range is preferably from 5 to 30% by weight based on the weight of NH 4 AlF 4 containing 6 . Below this range, the effect is small, and beyond this range, no remarkable effect is observed on the powder properties such as the average particle size and the bulk density. The seed crystal is preferably (NH 4 ) 3 AlF 6 from the viewpoint of purity.
【００１７】アンモニアは、ガス状でも液体状でも特に
限定されない。また反応時のｐＨは、中性付近が好まし
く、ｐＨが高いとアンモニアのロスとなり、また母液処
理及び環境面においても好ましくない。一方、ｐＨが低
いと反応するために必要なアンモニアが不足することに
なり反応が進行し難くなる。従って、純度が低くなり好
ましくない。Ammonia is not particularly limited, whether it is gaseous or liquid. The pH at the time of the reaction is preferably around neutral. If the pH is high, ammonia is lost, and it is not preferable in terms of mother liquor treatment and environmental aspects. On the other hand, if the pH is low, the ammonia required for the reaction becomes insufficient, and the reaction hardly proceeds. Therefore, the purity is undesirably low.
【００１８】反応温度は、４０〜９０℃の範囲が好まし
い。反応温度が低い場合、粒子径及び嵩密度が小さくな
り、純度も低下する。一方、９０℃以上においては、純
度及び粉体物性の改善は見られず加熱によるエネルギー
のロスとなる。[0018] The reaction temperature is preferably in the range of 40 to 90 ° C. When the reaction temperature is low, the particle size and bulk density are reduced, and the purity is also reduced. On the other hand, above 90 ° C., no improvement in purity and physical properties of the powder is observed, resulting in energy loss due to heating.
【００１９】このようにして得られた反応スラリーを固
液分離、洗浄、乾燥することによりＮＦ3の製造原料に
適した平均粒子径、嵩密度が大きく、かつ純度の高い
（ＮＨ4）3ＡｌＦ6を得ることができる。The thus-obtained reaction slurry is subjected to solid-liquid separation, washing and drying to obtain (NH 4 ) 3 AlF having a large average particle size, a large bulk density and a high purity suitable for a raw material for producing NF 3. You can get 6 .
【００２０】[0020]
【実施例】以下、実施例により本発明を具体的に説明す
るが、かかる実施例に限定されるものではない。EXAMPLES The present invention will be described below in more detail with reference to Examples, but it should not be construed that the invention is limited thereto.
【００２１】実施例１〜１２、比較例１〜６ １００ｌのポリテトラフルオロエチレン製の槽に水５０
Ｋｇと種晶として（ＮＨ4）3ＡｌＦ6を仕込み、攪拌し
ながら反応温度７０℃で種々の割合の（ＮＨ4） 3ＡｌＦ
6を含有するＮＨ4ＡｌＦ4１３Ｋｇを２０％フッ酸溶液
でスラリー化して反応槽へ１０時間で加えた。一方で
は、反応槽のｐＨを７±０．５に維持するように２５％
アンモニア水で調整した。反応スラリーは、固液分離
し、水洗後１５０℃で乾燥した。結果を表１、表２に示
した。尚、嵩密度は、ＪＩＳＫ５１０１により測定し
た。Examples 1 to 12 and Comparative Examples 1 to 6 Water was added to a 100 l polytetrafluoroethylene tank.
Kg and seed crystals (NHFour)ThreeAlF6Charge and stir
While the reaction temperature was 70 ° C., various proportions of (NHFour) ThreeAlF
6Containing NHFourAlFFour13 kg in 20% hydrofluoric acid solution
And added to the reaction vessel over 10 hours. On the other hand
Is 25% to maintain the pH of the reactor at 7 ± 0.5.
Adjusted with aqueous ammonia. Reaction slurry is separated into solid and liquid
Then, it was washed with water and dried at 150 ° C. The results are shown in Tables 1 and 2.
did. The bulk density was measured according to JIS K5101.
Was.
【００２２】[0022]
【表１】 [Table 1]
【００２３】[0023]
【表２】 [Table 2]
【００２４】[0024]
【発明の効果】本発明の方法により、三フッ化窒素の製
造原料となる、高純度で、嵩密度が高く、平均粒径の大
きなヘキサフルオロアルミニウムアンモニウムの製造を
可能にした。According to the method of the present invention, it is possible to produce hexafluoroaluminum ammonium having a high purity, a high bulk density and a large average particle size, which is a raw material for producing nitrogen trifluoride.
Claims (2)
ムを含有するテトラフルオロアルミニウムアンモニウム
のフッ酸溶液スラリーとアンモニアとを反応させる際
に、種晶をヘキサフルオロアルミニウムアンモニウムを
含有するテトラフルオロアルミニウムアンモニウムに対
して５〜３０重量％添加することを特徴とするヘキサフ
ルオロアルミニウムアンモニウムの製造方法。When reacting a hydrofluoric acid solution slurry of tetrafluoroaluminum ammonium containing hexafluoroaluminum ammonium with ammonia, a seed crystal is formed in an amount of 5 to 30 with respect to tetrafluoroaluminum ammonium containing hexafluoroaluminum ammonium. A method for producing hexafluoroaluminum ammonium, which is added by weight%.
ム中のヘキサフルオロアルミニウムアンモニウムの含有
量が５〜５０重量％の範囲であることを特徴とする請求
項１記載のヘキサフルオロアルミニウムアンモニウムの
製造方法。2. The method for producing hexafluoroaluminum ammonium according to claim 1, wherein the content of ammonium hexafluoroaluminum in the tetrafluoroaluminum ammonium is in the range of 5 to 50% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10351001A JP2000169141A (en) | 1998-12-10 | 1998-12-10 | Production of ammonium hexafluoroaluminate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10351001A JP2000169141A (en) | 1998-12-10 | 1998-12-10 | Production of ammonium hexafluoroaluminate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000169141A true JP2000169141A (en) | 2000-06-20 |
Family
ID=18414369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10351001A Pending JP2000169141A (en) | 1998-12-10 | 1998-12-10 | Production of ammonium hexafluoroaluminate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000169141A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005330207A (en) * | 2004-05-19 | 2005-12-02 | Mitsubishi Gas Chem Co Inc | Method for producing high purity spiroglycol with improved particle size |
| JP2006312570A (en) * | 2005-05-09 | 2006-11-16 | Central Glass Co Ltd | Producing method of ammonium cryolite |
| JP2007126448A (en) * | 2005-10-04 | 2007-05-24 | Mitsubishi Gas Chem Co Inc | Method for producing dioxane glycol |
| JP2007290918A (en) * | 2006-04-26 | 2007-11-08 | Central Glass Co Ltd | Method for producing ammonium cryolite |
| CN109052440A (en) * | 2018-08-08 | 2018-12-21 | 浙江大学 | A method of four ammonium aluminum fluorides of production and side product sodium chloride |
-
1998
- 1998-12-10 JP JP10351001A patent/JP2000169141A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005330207A (en) * | 2004-05-19 | 2005-12-02 | Mitsubishi Gas Chem Co Inc | Method for producing high purity spiroglycol with improved particle size |
| JP2006312570A (en) * | 2005-05-09 | 2006-11-16 | Central Glass Co Ltd | Producing method of ammonium cryolite |
| JP2007126448A (en) * | 2005-10-04 | 2007-05-24 | Mitsubishi Gas Chem Co Inc | Method for producing dioxane glycol |
| JP2007290918A (en) * | 2006-04-26 | 2007-11-08 | Central Glass Co Ltd | Method for producing ammonium cryolite |
| CN109052440A (en) * | 2018-08-08 | 2018-12-21 | 浙江大学 | A method of four ammonium aluminum fluorides of production and side product sodium chloride |
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