JP2844368B2 - Method for producing ceric ammonium nitrate - Google Patents
Method for producing ceric ammonium nitrateInfo
- Publication number
- JP2844368B2 JP2844368B2 JP1291983A JP29198389A JP2844368B2 JP 2844368 B2 JP2844368 B2 JP 2844368B2 JP 1291983 A JP1291983 A JP 1291983A JP 29198389 A JP29198389 A JP 29198389A JP 2844368 B2 JP2844368 B2 JP 2844368B2
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- Prior art keywords
- ammonium nitrate
- nitric acid
- cerium
- weight
- molar ratio
- Prior art date
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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
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- 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)
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。Description: TECHNICAL 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。Cerium ammonium nitrate is a compound useful as an oxidizing agent and a 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In
d.Eng.Chem.,Anal.Ed.,8,449（1936）及びTalanta 10,7
09（1963）等に記載されている。<Problems to be solved by the prior art and invention> Regarding the method for producing ceric ammonium nitrate, In
d.Eng.Chem., Anal.Ed., 8,449 (1936) and Talanta 10,7
09 (1963).
該方法は酸化セリウム（CeO2），酸化セリウム水和物
（CeO2・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 (CeO 2 ) and cerium oxide hydrate (CeO 2 .H 2 O) are 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 this method relates to a method for producing ceric ammonium nitrate as a reagent for analysis, a high purity product can be obtained, but there is a problem that the yield is low.
すなわち、第１次晶の収率は約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次晶、第３次晶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。That is, the yield of the primary crystal is about 60%, and the purity is 99.4% by weight. For this reason, in order to increase the yield, it is necessary to further recover the secondary crystal and the tertiary crystal, and the recovery operation is 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次晶の収率が高く、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 such circumstances, the present inventors have conducted intensive studies,
The present inventors have found a method for producing ceric ammonium nitrate having a high yield of primary crystals and a simple crystallization operation, and have conducted various studies to complete the present invention.
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を提供するものである。That is, the present invention relates to a method for producing ceric ammonium nitrate by dissolving cerium oxide, cerium oxide hydrate or cerium hydroxide with nitric acid, adding ammonium nitrate to the solution, A method for producing ceric ammonium nitrate using nitric acid having a nitric acid concentration of 50% by weight or more, wherein nitric acid / cerium (molar ratio) is 4 or more and ammonium nitrate / cerium (molar ratio) is 1.5 or more. To provide.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
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 material used in the present invention is 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. It is not preferable to include a reducing element such as iron and manganese. The mixing of water is not particularly limited.
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 a raw material such as cerium oxide is dissolved in nitric acid, nitric acid is used, which has a nitric acid concentration of 50% by weight or more in a reaction system at the time of charging the raw material.
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。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。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 the raw material such as cerium oxide, the method of the present invention defines the nitric acid concentration in the reaction system at the time of charging the raw material. is there. In the method of the present invention, it is preferable to use nitric acid which has a nitric acid concentration of 52 to 90% by weight in the reaction system at the time of charging the raw materials.
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。通常該モル比は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。In the method of the present invention, the molar ratio of nitric acid / cerium is 4 or more, and the upper limit is not particularly limited. As for the upper limit, an economical point may be appropriately determined depending on the relationship between the amount of raw materials used and the yield. Usually, the molar ratio is set in the range of 4 to 40. More preferably, the molar ratio is in the range of 6-20.
酸化セリウム等を硝酸に溶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℃である。The reaction temperature for dissolving cerium oxide or the like in nitric acid may be a temperature equal to or lower than 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。The reaction time at this time is appropriately determined depending on the type of the raw material, the nitric acid concentration and the 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。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
該モル比は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。According to the method of the present invention, ammonium nitrate is added to the cerium nitric acid solution obtained as described above, and ammonium nitrate / cerium (molar ratio) = 1.5 or more. The upper limit of the molar ratio is not particularly limited, and an economical point may be appropriately determined depending on the amount of the raw material used and the yield. Usually, the molar ratio is set in the range of 1.5 to 10. More preferably, the molar ratio is in the range of 2-6.
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併せられる。In the present invention, by setting the concentration and amount of nitric acid and the amount of ammonium nitrate in the reaction system at the time of charging the raw materials in specific ranges, ceric ammonium nitrate can be obtained as crystals in high yield. The obtained ceric ammonium nitrate is separated by filtration and separated from the reaction solution, and then used for drying 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℃である。The reaction temperature when using ammonium nitrate may be a temperature lower than 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 the raw material 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 described in detail 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 charging the raw materials are respectively specified, thereby achieving higher results than 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> Hereinafter, the present invention will be described 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 Cerium hydroxide (purity 77.6% by weight, moisture 20.9% by weight)
55g% nitric acid is added to 5g, nitric acid / cerium (molar ratio)
= 9.36 and stirred at 80 ° C for 60 minutes. The nitric acid concentration in the reaction system at the time of charging the raw materials was 52.3% 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、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。Further, ammonium nitrate was added to the solution to make ammonium nitrate / cerium (molar ratio) = 3.71.
After stirring for 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 its 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℃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 To 5 g of cerium hydroxide as in Example 1, 61% by weight of nitric acid was added to make nitric acid / cerium (molar ratio) = 7.97.
Stirred for 60 minutes. The concentration of nitric acid 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℃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) = 2.74.
After stirring for 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 the 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℃
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 To 5 g of cerium hydroxide as in Example 1, 69.3% by weight of nitric acid was added, and nitric acid / cerium (molar ratio) was set to 9.05.
For 60 minutes. 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℃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.
After stirring for 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 of nitric acid was added to 5 g of cerium hydroxide in the same manner as in Example 1 to make nitric acid / cerium (molar ratio) = 12.4.
Stirred for 60 minutes. 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。Further, ammonium nitrate was added to the solution, and ammonium nitrate / cerium (molar ratio) was set to 2.71.
After stirring for 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 its 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℃
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 of nitric acid was added to 5 g of cerium hydroxide in the same manner as in Example 1 to make nitric acid / cerium (molar ratio) = 12.3, and 80 ° C.
For 60 minutes. 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℃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.
After stirring for 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 the 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℃
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 To 5 g of cerium hydroxide as in Example 1, 67.5% by weight of nitric acid was added to make nitric acid / cerium (molar ratio) = 4.88, and 80 ° C.
For 60 minutes. 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℃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, and ammonium nitrate / cerium (molar ratio) was set to 2.71.
After stirring for 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 the purity was 98.3% by weight.
実施例７ 表面積145m2/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℃で４時間撹拌した。Example 7 5 g of cerium oxide having a surface area of 145 m 2 / g and a purity of 99.9% by weight
69.3 wt% nitric acid, nitric acid / cerium (molar ratio)
= 7.58 and 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℃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。Further, the insoluble matter was filtered off, and ammonium nitrate was added to the filtrate, and ammonium nitrate / cerium (molar ratio) = 1.74.
And stirred at 50 ° C. for 30 minutes, then cooled, filtered and dried,
Cerium ammonium nitrate was 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 the purity was 99.3% by weight.
実施例８ 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℃
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 8 To 5 g of cerium hydroxide as in Example 1, 69.3% by weight of nitric acid was added to make nitric acid / cerium (molar ratio) = 9.05,
For 30 minutes. 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℃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 stirred at 80 ° C. for 10 minutes, then 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48.8重量％）
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, water 48.8% by weight)
To 5 g, 69.3% by weight of nitric acid was added to adjust nitric acid / cerium (molar ratio) to 19.04, and the mixture was stirred at 60 ° C. for 3 hours. 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℃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。Further, ammonium nitrate was added to the solution to make ammonium nitrate / cerium (molar ratio) = 5.84.
After stirring for 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 the 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℃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 To 5 g of cerium hydroxide as in Example 1, 40% by weight of nitric acid was added, and nitric acid / cerium (molar ratio) was set to 8.51.
Stirred for 60 minutes. 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、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。Further, ammonium nitrate was added to the solution to make ammonium nitrate / cerium (molar ratio) = 2.71.
After stirring for 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重量％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% by weight of nitric acid was added to make nitric acid / cerium (molar ratio) = 3.74.
Stir for 30 minutes. The concentration of nitric acid 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℃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。Further, ammonium nitrate was added to the solution to make ammonium nitrate / cerium (molar ratio) = 2.71.
After stirring for 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 the 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℃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 of nitric acid was added to 5 g of cerium hydroxide as in Example 1 to make nitric acid / cerium (molar ratio) = 8.58.
Stirred for 60 minutes. The concentration of nitric acid 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。Further, ammonium nitrate was added to the solution to make ammonium nitrate / cerium (molar ratio) = 1.34.
After stirring for 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.
フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C01F 17/00 C01C 1/18 C01C 1/28Continuation of front page (58) Field surveyed (Int.Cl. 6 , DB name) C01F 17/00 C01C 1/18 C01C 1/28
Claims (1)
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ニウムを製造す
る方法において、原料仕込み時の反応系中の硝酸濃度が
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。1. A method for producing ceric ammonium nitrate by dissolving cerium oxide, cerium oxide hydrate or cerium hydroxide with nitric acid, and adding ammonium nitrate to the solution, the method comprising the steps of: Nitric acid concentration
Using nitric acid of 50% by weight or more, nitric acid / cerium (molar ratio) is 4 or more, and ammonium nitrate / cerium (molar ratio).
The method for producing ceric ammonium nitrate, wherein the 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 JPH03153520A (en) | 1991-07-01 |
| JP2844368B2 true 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928420A (en) * | 2019-04-11 | 2019-06-25 | 四川沃耐稀新材料科技有限公司 | The production technology of electronic grade nitric acid cerium ammonium |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2742353B1 (en) * | 1995-12-13 | 1998-01-09 | Commissariat Energie Atomique | PROCESS FOR ELECTROCATALYTIC REDUCING DISSOLUTION OF CERIUM REFRACTORY COMPOUNDS |
| 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 producing 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 |
| 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 of recovering nitric acid from chromium etching waste solution and producing cerium ammonium nitride |
-
1989
- 1989-11-08 JP JP1291983A patent/JP2844368B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928420A (en) * | 2019-04-11 | 2019-06-25 | 四川沃耐稀新材料科技有限公司 | The production technology of electronic grade nitric acid cerium ammonium |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03153520A (en) | 1991-07-01 |
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