JPH03153520A - Production of ceric ammonium nitrate - Google Patents
Production of ceric ammonium nitrateInfo
- Publication number
- JPH03153520A JPH03153520A JP1291983A JP29198389A JPH03153520A JP H03153520 A JPH03153520 A JP H03153520A JP 1291983 A JP1291983 A JP 1291983A JP 29198389 A JP29198389 A JP 29198389A JP H03153520 A JPH03153520 A JP H03153520A
- Authority
- JP
- Japan
- Prior art keywords
- ammonium nitrate
- nitric acid
- cerium
- weight
- molar ratio
- 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
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 60
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 34
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 claims abstract description 15
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 9
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 9
- KKFPIBHAPSRIPB-UHFFFAOYSA-N cerium(3+);oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Ce+3].[Ce+3] KKFPIBHAPSRIPB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 25
- 238000007796 conventional method Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 239000007858 starting material Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- OSUPRVCFDQWKQN-UHFFFAOYSA-N cerium;nitric acid Chemical compound [Ce].O[N+]([O-])=O.O[N+]([O-])=O.O[N+]([O-])=O.O[N+]([O-])=O.O[N+]([O-])=O.O[N+]([O-])=O OSUPRVCFDQWKQN-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は複雑な工程を必要とせずに高収率で硝酸第二セ
リウムアンモニウムを製造する方法に関するものである
。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing ceric ammonium nitrate in high yield without requiring complicated steps.
硝酸第二セリウムアンモニウムは酸化剤、触媒として有
機合成その他の分野に有用な化合物である。Ceric ammonium nitrate is a compound useful as an oxidizing agent and catalyst in organic synthesis and other fields.
〈従来の技術及び発明が解決しようとする課題〉硝酸第
二セリウムアンモニウムの製造法に関してはＩｎｄ、Ｅ
ｎｇ、Ｃｈｅｍ、、Ａｎａｌ、Ｅｄ、、８．４４９（１
９３６）及びＴａ１ａｎｔａ １０，７０９（１９６３
）等に記載されている。<Prior art and problems to be solved by the invention> Regarding the production method of ceric ammonium nitrate, Ind.
ng,Chem,,Anal,Ed,,8.449(1
936) and Ta1anta 10,709 (1963
) etc.
該方法は酸化セリウム（ＣｅＯｚ） ＋酸化セリウム水
和物（Ｃｅｎｔ・Ｈ２Ｏ）を熱濃硝酸に溶解し、次いで
硝酸アンモニウムを添加して硝酸第二セリウムアンモニ
ウムを製造している。In this method, cerium oxide (CeOz) + cerium oxide hydrate (Cent.H2O) is dissolved in hot concentrated nitric acid, and then ammonium nitrate is added to produce ceric ammonium nitrate.
しかしながら該方法は分析用試薬としての硝酸第二セリ
ウムアンモニウムの製造方法に関するものであるため、
純度の高いものが得られるが、収率が低いという課題を
有している。However, since the method is related to a method for producing ceric ammonium nitrate as an analytical reagent,
Although a product with high purity can be obtained, the problem is that the yield is low.
すなわち、第１成品の収率は約６０％、純度は９９．４
重量％である。このため、収率を上げようとすると、さ
らに第２成品、第３成品と回収する必要があり、その回
収操作は一層煩雑なものである。In other words, the yield of the first product is approximately 60%, and the purity is 99.4.
Weight%. Therefore, in order to increase the yield, it is necessary to collect the second product and the third product, making the collection operation even more complicated.
〈課題を解決するための手段〉
かかる事情に鑑み、本発明者らは鋭意検討した結果、第
１成品の収率が高く、しかも結晶化操作が簡単な硝酸第
二セリウムアンモニウムの製造法を見出すとともに種々
の検討を加え本発明を完成させた。<Means for Solving the Problems> In view of the above circumstances, the inventors of the present invention have conducted extensive studies and have found a method for producing ceric ammonium nitrate that provides a high yield of the first product and that is easy to crystallize. The present invention was completed after various studies.
すなわち、本発明は酸化セリウム、酸化セリウム水和物
または水酸化セリウムを硝酸で溶解し、該溶液に硝酸ア
ンモニウムを添加して硝酸第二セリウムアンモラムを製
造する方法において、原料仕込み時の反応系内の硝酸濃
度が５０重憧％以上となる硝酸を用い、硝酸／セリウム
（モル比）を４以上、硝酸アンモニウム／セリウム（モ
ル比）を１．５以上とすることを特徴とする硝酸第二セ
リウムアンモニウムの製造法を提供するものである。That is, the present invention provides a method for producing ceric ammorum nitrate by dissolving cerium oxide, cerium oxide hydrate, or cerium hydroxide in nitric acid, and adding ammonium nitrate to the solution. Ceric ammonium nitrate characterized by using nitric acid with a nitric acid concentration of 50% or more, and having a nitric acid/cerium (molar ratio) of 4 or more and an ammonium nitrate/cerium (molar ratio) of 1.5 or more. The present invention provides a method for manufacturing.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明に用いる原料は酸化セリウム、酸化セリウム水和
物または水酸化セリウムであり、これらの原料中にはラ
ンタン、プラセオジム、ネオジム等のセリウム以外の希
土類元素が含まれていてもよい。なお、鉄、マンガン等
の還元性の元素が含まれるのは好ましくない、また水分
の混入については特に限定されるものではない。The raw materials used in the present invention are cerium oxide, cerium oxide hydrate, or cerium hydroxide, and these raw materials may contain rare earth elements other than cerium, such as lanthanum, praseodymium, and neodymium. Note that it is not preferable that reducing elements such as iron and manganese be included, and there are no particular limitations on the inclusion of water.
本発明方法は酸化セリウム等の原料を硝酸に溶解する際
に、原料仕込み時の反応系内の硝酸濃度が５０重量％以
上となる硝酸を用いることを特徴とする。The method of the present invention is characterized in that when dissolving raw materials such as cerium oxide in nitric acid, nitric acid is used so that the nitric acid concentration in the reaction system at the time of charging the raw materials is 50% by weight or more.
すなわち、酸化セリウム等の原料中の水分量の変動によ
り、反応系中の硝酸の濃度が変動するという不都合を有
するため、本発明方法は原料仕込み時の反応系内の硝酸
濃度を規定したものである。That is, since there is a disadvantage that the concentration of nitric acid in the reaction system fluctuates due to fluctuations in the amount of water in raw materials such as cerium oxide, the method of the present invention does not specify the concentration of nitric acid in the reaction system at the time of charging the raw materials. be.
本発明方法は原料仕込み時の反応系内の硝酸濃度が５２
〜９０重量％となる硝酸を用いるのが好ましい。In the method of the present invention, the nitric acid concentration in the reaction system at the time of charging raw materials is 52
It is preferable to use nitric acid of up to 90% by weight.
本発明方法は硝酸／セリウム（モル比）を４以上とし、
上限については特に限定されるものではない。その上限
については原料使用量、収率との関係により経済的な点
を適宜決定すればよい。通常咳モル比は４〜４０の範囲
で設定される。より好ましくは該モル比は６〜２０の範
囲がよい。The method of the present invention uses nitric acid/cerium (molar ratio) of 4 or more,
The upper limit is not particularly limited. The upper limit may be appropriately determined based on economic considerations in relation to the amount of raw materials used and the yield. Usually the cough molar ratio is set in the range of 4-40. More preferably, the molar ratio is in the range of 6 to 20.
酸化セリウム等を硝酸に熔解する際の反応温度は、その
系の沸点以下の温度でよく、通常５０〜１３０°Ｃであ
る。The reaction temperature for dissolving cerium oxide etc. in nitric acid may be a temperature below the boiling point of the system, and is usually 50 to 130°C.
またこの際の反応時間は原料の種類、硝酸濃度および反
応温度によって適宜決定される。Further, the reaction time at this time is appropriately determined depending on the type of raw materials, nitric acid concentration, and reaction temperature.
本発明方法は以上のようにして得たセリウムの硝酸溶液
に硝酸アンモニウムを加え、硝酸アンモニウム／セリウ
ム（モル比）−１，５以上とする。In the method of the present invention, ammonium nitrate is added to the cerium nitric acid solution obtained as described above to obtain an ammonium nitrate/cerium (molar ratio) of -1.5 or more.
該モル比の上限については特に限定されるものではなく
、原料使用量、収率との関係により経済的な点を適宜決
定すればよい、通常液モル比は１．５〜１０の範囲で設
定される。より好ましくは該モル比は２〜６の範囲がよ
い。The upper limit of the molar ratio is not particularly limited, and may be appropriately determined based on economic considerations in relation to the amount of raw materials used and the yield. The liquid molar ratio is usually set in the range of 1.5 to 10. be done. More preferably, the molar ratio is in the range of 2 to 6.
本発明は原料仕込み時の反応系内の硝酸の濃度、量およ
び硝酸アンモニウムの量を特定の範囲とすることにより
、硝酸第二セリウムアンモニウムを結晶として高収率で
得ることができる。得られた硝酸第二セリウムアンモニ
ウムは濾別され、反応液と分離された後、乾燥あるいは
未乾燥なまま使用に供せられる。In the present invention, ceric ammonium nitrate can be obtained in high yield as crystals by controlling the concentration and amount of nitric acid and the amount of ammonium nitrate within specific ranges in the reaction system when charging raw materials. The obtained ceric ammonium nitrate is filtered and separated from the reaction solution, and then used dry or undried.
また硝酸アンモニウムを用いる際の反応温度は、その系
の沸点以下の温度でよく、通常２５〜１３０°Ｃである
。Further, the reaction temperature when using ammonium nitrate may be a temperature below the boiling point of the system, and is usually 25 to 130°C.
さらに反応時間は原料の種類、反応温度により適宜決定
される。Further, the reaction time is appropriately determined depending on the type of raw materials and the reaction temperature.
〈発明の効果〉
以上詳述したように本発明方法によれば、原料仕込み時
の反応系内の硝酸濃度、量および硝酸アンモニウムの量
をそれぞれ特定のものとすることにより、従来の方法よ
りも高収率でしかも、作業性よく硝酸第二セリウムアン
モニウムを製造することができるのであるから、その工
業的価値は頗る大である。<Effects of the Invention> As detailed above, according to the method of the present invention, the concentration and amount of nitric acid and the amount of ammonium nitrate in the reaction system at the time of raw material preparation are set to specific values, thereby achieving a higher concentration than in the conventional method. Since ceric ammonium nitrate can be produced with high yield and good workability, its industrial value is extremely large.
〈実施例〉
以下、本発明を実施例により説明するが、本発明はこれ
ら実施例に限定されるものではない。<Examples> The present invention will be described below with reference to Examples, but the present invention is not limited to these Examples.
実施例１
水酸化セリウム（純度７７．６重量％、水分２０．９重
量％）５ｇに、５５重量％硝酸を加え、硝酸／セリウム
（モル比） ＝９．３６とし、８０℃で６０分間撹拌し
た。なお、原料仕込み時の反応系内の硝酸濃度は５２．
３重量％であった。Example 1 55% by weight nitric acid was added to 5g of cerium hydroxide (purity 77.6% by weight, moisture 20.9% by weight) to make nitric acid/cerium (molar ratio) = 9.36, and stirred at 80°C for 60 minutes. did. The nitric acid concentration in the reaction system at the time of charging raw materials was 52.
It was 3% by weight.
さらに、・該溶解液に硝酸アンモニウムを加え、硝酸ア
ンモニウム／セリウム（モル比） ＝３．７１とし、８
０゛Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝
酸第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 3.71, and 8
After stirring at 0°C for 10 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
７８．１％、その純度は９６．５重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 78.1%, and the purity was 96.5% by weight.
実施例２
実施例１と同様の水酸化セリウム５ｇに、６１重量％硝
酸を加え、硝酸／セリウム（モル比）−７，９７とし、
８０°Ｃで６０分間撹拌した。なお原料仕込み時の反応
系内の硝酸濃度は５７．０重量％であった。Example 2 61% by weight nitric acid was added to 5 g of cerium hydroxide similar to Example 1 to give a nitric acid/cerium (molar ratio) of -7.97,
Stirred at 80°C for 60 minutes. The nitric acid concentration in the reaction system at the time of charging the raw materials was 57.0% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） −２，７４とし、８０
゛Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) -2.74, and 80
After stirring for 10 minutes at °C, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
９１．７％、その純度は９７．１重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 91.7%, and its purity was 97.1% by weight.
実施例３
実施例１と同様の水酸化セリウム５ｇに、６９．３重量
％硝酸を加え、硝酸／セリウム（モル比）＝９．０５と
し、８０°Ｃで６０分間撹拌した。なお、原料仕込み時
の反応系内の硝酸濃度は６４．８重量％であった。Example 3 69.3% by weight nitric acid was added to 5 g of cerium hydroxide as in Example 1 to give a nitric acid/cerium (molar ratio) of 9.05, and the mixture was stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 64.8% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝２．７８とし、８０
°Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 2.78, and 80
After stirring at °C for 10 minutes, it was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
９４．８％、その純度は９７．７重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 94.8%, and the purity was 97.7% by weight.
実施例４
実施例１と同様の水酸化セリウム５ｇに、７３重量％硝
酸を加え、硝酸／セリウム（モル比）＝１２．４とし、
８０℃で６０分間撹拌した。なお、原料仕込み時の反応
系内の硝酸濃度は６９．４重量％であった。Example 4 73% by weight nitric acid was added to 5 g of cerium hydroxide similar to Example 1 to make nitric acid/cerium (molar ratio) = 12.4,
Stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 69.4% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比＞ ＝２．７１．１！：し
、８０°Ｃで１０分間撹拌した後、冷却、濾過、乾燥し
、硝酸第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution, ammonium nitrate/cerium (molar ratio >=2.71.1!) was stirred at 80°C for 10 minutes, and then cooled, filtered, and dried to obtain ceric ammonium nitrate. Obtained.
分析した結果、硝酸第二セリウムアンモニウムの収率は
８４．７％、その純度は９７．１重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 84.7%, and the purity was 97.1% by weight.
実施例５
実施例１と同様の水酸化セリウム５ｇに、９４．１重量
％硝酸を加え、硝酸／セリウム（モル比）＝１２．３と
し、８０°Ｃで６０分間撹拌した。なお、原料仕込み時
の反応系内の硝酸濃度は８８．０重量％であった。Example 5 94.1% by weight nitric acid was added to 5 g of the same cerium hydroxide as in Example 1 to give a nitric acid/cerium (molar ratio) of 12.3, and the mixture was stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 88.0% by weight.
さらに、該熔解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝２．７８とし、８０
°Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the melt to make ammonium nitrate/cerium (molar ratio) = 2.78, and 80
After stirring at °C for 10 minutes, it was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
７６．９％、その純度は８３．１重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 76.9%, and its purity was 83.1% by weight.
実施例６
実施例１と同様の水酸化セリウム５ｇに、６７．５重量
％硝酸を加え、硝酸／セリウム（モル比）＝４．８８と
し、８０゛Ｃで６０分間撹拌した。なお、原料仕込み時
の反応系内の硝酸濃度は６０．１重量％であった。Example 6 67.5% by weight nitric acid was added to 5 g of cerium hydroxide as in Example 1 to give a nitric acid/cerium (molar ratio) of 4.88, and the mixture was stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 60.1% by weight.
さらに、該熔解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝２．７１とし、８０
“Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the melt to make ammonium nitrate/cerium (molar ratio) = 2.71, and 80
After stirring at C for 10 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
７２．１％、その純度は９８．３重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 72.1%, and its purity was 98.3% by weight.
実施例７
表面積１４５ｒｄ／ｇ、純度９９．９重量％の酸化セリ
ウム５ｇに、６９．３重量％硝酸を加え、硝酸／セリウ
ム（モル比） ＝７．５８とし、１３０°Ｃで４時間撹
拌した。Example 7 69.3% by weight nitric acid was added to 5g of cerium oxide with a surface area of 145rd/g and a purity of 99.9% by weight to make nitric acid/cerium (molar ratio) = 7.58, and the mixture was stirred at 130°C for 4 hours. .
さらに、不溶解分を濾別し、濾液に硝酸アンモニウムを
加え、硝酸アンモニウム／セリウム（モル比） ＝１．
７４とし、５０゛Ｃで３０分間撹拌した後、冷却、濾過
、乾燥し、硝酸第二セリウムアンモニウムを得た。Furthermore, insoluble matter was filtered out, and ammonium nitrate was added to the filtrate to give ammonium nitrate/cerium (molar ratio) = 1.
After stirring at 50°C for 30 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
７８．０％、その純度は９９．３重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 78.0%, and its purity was 99.3% by weight.
実施例日
実施例１と同様の水酸化セリウム５ｇに、６９．３重量
％硝酸を加え、硝酸／セリウム（モル比）＝９．０５と
し、８０°Ｃで３０分間撹拌した。なお、原料仕込み時
の反応系内の硝酸濃度は６４．８重量％であった。Example Day 69.3% by weight nitric acid was added to 5 g of cerium hydroxide as in Example 1 to give a nitric acid/cerium (molar ratio) of 9.05, and the mixture was stirred at 80°C for 30 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 64.8% by weight.
さらに該溶解液に硝酸アンモニウムを加え、硝酸アンモ
ニウム／セリウム（モル比） ＝２．７８とし、８０°
Ｃで１０分間撹拌した後、冷却、濾過、乾燥し、硝酸第
二セリウムアンモニウムを得た。Further, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 2.78, and the mixture was heated at 80°
After stirring at C for 10 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
９６．１％、その純度は９７．０重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 96.1%, and the purity was 97.0% by weight.
実施例９
水酸化セリウム（純度３６．１重量％、水分４Ｂ、８．
１景％）５ｇに、６９．３重量％硝酸を加え、硝酸／セ
リウム（モル比） ＝ １９．０４とし、６０℃で３時
間撹拌した。なお、原料仕込み時の反応系内の硝酸濃度
は５９．６重量％であった。Example 9 Cerium hydroxide (purity 36.1% by weight, moisture 4B, 8.5% by weight)
69.3% by weight of nitric acid was added to 5g of cerium (nitric acid/cerium (molar ratio) = 19.04), and the mixture was stirred at 60°C for 3 hours. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 59.6% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝５．８４とし、６０
°Ｃで３０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 5.84, and 60
After stirring at °C for 30 minutes, it was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
９７．７％、その純度は９７．９重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 97.7%, and its purity was 97.9% by weight.
比較例１
実施例１と同様の水酸化セリウム５ｇに、４０重量％硝
酸を加え、硝酸／セリウム（モル比）＝８．５１とし、
８０°Ｃで６０分間撹拌した。なお、原料仕込み時の反
応系内の硝酸濃度は３８．４重量％であった。Comparative Example 1 40% by weight nitric acid was added to 5 g of cerium hydroxide similar to Example 1 to make nitric acid/cerium (molar ratio) = 8.51,
Stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 38.4% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝２．７１とし、８
０℃で１０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 2.71, and 8
After stirring at 0° C. for 10 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
２．１％、その純度は９９．８重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 2.1%, and its purity was 99.8% by weight.
比較例２
実施例１と同様の水酸化セリウム５ｇに、８０重重景硝
酸を加え、硝酸／セリウム（モル比）＝３．７４とし、
８０℃で３０分間撹拌した。なお、原料仕込み時の反応
系内の硝酸濃度は６７．２重量％であった。Comparative Example 2 To 5 g of cerium hydroxide similar to that in Example 1, 80 heavy bicarbonate of nitric acid was added to make nitric acid/cerium (molar ratio) = 3.74,
Stirred at 80°C for 30 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 67.2% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝２．７１とし、８０
°Ｃで３０分間撹拌した後、冷却、濾過、乾燥し、硝酸
第二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 2.71, and 80
After stirring at °C for 30 minutes, it was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
５７，８％、その純度は９５．６重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 57.8%, and its purity was 95.6% by weight.
比較例３
実施例１と同様の水酸化セリウム５ｇに、７２重量％硝
酸を加え、硝酸／セリウム（モル比）＝８．５８とし、
８０゛ｃで６０分間撹拌した。なお、原料仕込み時の反
応系内の硝酸濃度は６７．０重量％であった。Comparative Example 3 72% by weight nitric acid was added to 5 g of cerium hydroxide similar to Example 1 to make nitric acid/cerium (molar ratio) = 8.58,
The mixture was stirred at 80°C for 60 minutes. Note that the nitric acid concentration in the reaction system at the time of charging the raw materials was 67.0% by weight.
さらに、該溶解液に硝酸アンモニウムを加え、硝酸アン
モニウム／セリウム（モル比） ＝１．３４とし、８０
℃で１０分間撹拌した後、冷却、濾過、乾燥し、硝酸第
二セリウムアンモニウムを得た。Furthermore, ammonium nitrate was added to the solution to make ammonium nitrate/cerium (molar ratio) = 1.34, and 80
After stirring at °C for 10 minutes, the mixture was cooled, filtered, and dried to obtain ceric ammonium nitrate.
分析した結果、硝酸第二セリウムアンモニウムの収率は
６３．９％、その純度は９８．２重量％であった。As a result of analysis, the yield of ceric ammonium nitrate was 63.9%, and its purity was 98.2% by weight.
Claims (1)
ムを硝酸で溶解し、該溶液に硝酸アンモニウムを添加し
て硝酸第二セリウムアンモニウムを製造する方法におい
て、原料仕込み時の反応系内の硝酸濃度が５０重量％以
上となる硝酸を用い、硝酸／セリウム（モル比）を４以
上、硝酸アンモニウム／セリウム（モル比）を１．５以
上とすることを特徴とする硝酸第二セリウムアンモニウ
ムの製造法。In a method for producing ceric ammonium nitrate by dissolving cerium oxide, cerium oxide hydrate, or cerium hydroxide in nitric acid and adding ammonium nitrate to the solution, the nitric acid concentration in the reaction system at the time of raw material charging is 50% by weight. % or more, nitric acid/cerium (molar ratio) is 4 or more, and ammonium nitrate/cerium (molar ratio) is 1.5 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291983A JP2844368B2 (en) | 1989-11-08 | 1989-11-08 | Method for producing ceric ammonium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1291983A JP2844368B2 (en) | 1989-11-08 | 1989-11-08 | Method for producing ceric ammonium nitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03153520A true JPH03153520A (en) | 1991-07-01 |
| JP2844368B2 JP2844368B2 (en) | 1999-01-06 |
Family
ID=17775995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1291983A Expired - Fee Related JP2844368B2 (en) | 1989-11-08 | 1989-11-08 | Method for producing ceric ammonium nitrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2844368B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2308130A (en) * | 1995-12-13 | 1997-06-18 | Commissariat Energie Atomique | Electrocatalytic reducing dissolving of refractory compounds of cerium |
| GB2328447A (en) * | 1997-08-16 | 1999-02-24 | British Aerospace | A desmutting solution for use prior to anodising |
| JP2002068741A (en) * | 2000-08-24 | 2002-03-08 | Asahi Kagaku Kogyo Co Ltd | Method for manufacturing cerium (iv) ammonium nitrate |
| KR20020022309A (en) * | 2000-09-19 | 2002-03-27 | 정지완 | Ceric ammonium nitrate manufacture method |
| JP2002220229A (en) * | 2001-01-18 | 2002-08-09 | Sumitomo Chem Co Ltd | Method for producing ammonium cerium (iv) nitrate |
| KR100391715B1 (en) * | 2000-10-05 | 2003-07-16 | 일동화학 주식회사 | Method for preparing ceric ammonium nitrate with high purity |
| KR100605365B1 (en) * | 2004-12-23 | 2006-07-31 | 재단법인 포항산업과학연구원 | Method for manufacturing cerium ammonium nitrate and withdrawing nitric acid from waste chrome etching solution |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928420B (en) * | 2019-04-11 | 2020-06-16 | 四川沃耐稀新材料科技有限公司 | Production process of electronic grade ammonium ceric nitrate |
-
1989
- 1989-11-08 JP JP1291983A patent/JP2844368B2/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2308130A (en) * | 1995-12-13 | 1997-06-18 | Commissariat Energie Atomique | Electrocatalytic reducing dissolving of refractory compounds of cerium |
| US5830342A (en) * | 1995-12-13 | 1998-11-03 | Commissariat A L'energie Atomique | Process for the electrocatalytic reducing dissolving of refractory compounds of cerium |
| GB2308130B (en) * | 1995-12-13 | 1999-06-16 | Commissariat Energie Atomique | Process for the electrocatalytic reducing dissolving of refractory compounds of cerium |
| GB2328447A (en) * | 1997-08-16 | 1999-02-24 | British Aerospace | A desmutting solution for use prior to anodising |
| JP2002068741A (en) * | 2000-08-24 | 2002-03-08 | Asahi Kagaku Kogyo Co Ltd | Method for manufacturing cerium (iv) ammonium nitrate |
| KR20020022309A (en) * | 2000-09-19 | 2002-03-27 | 정지완 | Ceric ammonium nitrate manufacture method |
| KR100391715B1 (en) * | 2000-10-05 | 2003-07-16 | 일동화학 주식회사 | Method for preparing ceric ammonium nitrate with high purity |
| JP2002220229A (en) * | 2001-01-18 | 2002-08-09 | Sumitomo Chem Co Ltd | Method for producing ammonium cerium (iv) nitrate |
| JP4742422B2 (en) * | 2001-01-18 | 2011-08-10 | 住友化学株式会社 | Method for producing cerium (IV) ammonium nitrate |
| KR100605365B1 (en) * | 2004-12-23 | 2006-07-31 | 재단법인 포항산업과학연구원 | Method for manufacturing cerium ammonium nitrate and withdrawing nitric acid from waste chrome etching solution |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2844368B2 (en) | 1999-01-06 |
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