JP2010174352A - Method for producing rhodium black - Google Patents

Method for producing rhodium black Download PDF

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JP2010174352A
JP2010174352A JP2009020705A JP2009020705A JP2010174352A JP 2010174352 A JP2010174352 A JP 2010174352A JP 2009020705 A JP2009020705 A JP 2009020705A JP 2009020705 A JP2009020705 A JP 2009020705A JP 2010174352 A JP2010174352 A JP 2010174352A
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rhodium
nitrite
ammonium
added
black
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Satoshi Okada
智 岡田
Shintaro Nakaie
新太郎 仲家
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Mitsubishi Materials Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing rhodium black from ammonium rhodium nitrite without generating NOx and further increasing a load to water treatment. <P>SOLUTION: The method for producing rhodium black is characterized in that water and an ammonium salt are added to an ammonium rhodium nitrite solution or a solution of the salt thereof, heating is performed, further, its pH is adjusted to a strong acid range so as to produce rhodium chloride nitrite, next, formic acid is added, and the rhodium chloride nitrite is reduced so as to produce metal rhodium (rhodium black). Preferably, the decomposing temperature of the ammonium rhodium nitrite is controlled to 60 to 80°C, and its pH is adjusted to 1 to 2. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、イオン交換法などで回収した亜硝酸ロジウムアンモニウムからロジウムブラック（ロジウム粉末）を効率良く製造する方法に関する。   The present invention relates to a method for efficiently producing rhodium black (rhodium powder) from rhodium ammonium nitrite recovered by an ion exchange method or the like.

自動車の排ガス制御用触媒などからロジウムを回収する方法として、イオン交換法によって不純物などを除去することにより亜硝酸ロジウムアンモニウムを回収し、この亜硝酸ロジウムアンモニウムからロジウムブラックを製造する技術が知られている。   As a method of recovering rhodium from automobile exhaust gas control catalysts, etc., a technique for recovering rhodium ammonium nitrite by removing impurities by ion exchange method and producing rhodium black from this rhodium ammonium nitrite is known. Yes.

具体的には、図２のフローに示すように、先ず、亜硝酸ロジウムアンモニウム塩に水と濃塩酸を添加し、８０℃程度に加熱した後、室温に達するまで放冷することにより、塩化ロジウム水溶液とし、次いで、これに塩化アンモニウムを添加して塩化ロジウムアンモニウムを生成する。この塩化ロジウムアンモニウムの溶解度が大きいので、エタノールを加えた後に、濾過して塩化ロジウムアンモニウムを回収する。この回収した沈殿物に水を加え、さらにギ酸を加えて８０℃に加熱し、ｐＨ４程度の液性下で、塩化ロジウムアンモニウムを還元してロジウムブラック（金属ロジウム微粒子）を析出させ、これを濾過してロジウムブラックを回収する。   Specifically, as shown in the flow of FIG. 2, first, water and concentrated hydrochloric acid are added to rhodium nitrite ammonium salt, heated to about 80 ° C., and then allowed to cool to room temperature, thereby rhodium chloride. An aqueous solution is then added to which ammonium chloride is added to produce rhodium ammonium chloride. Since this rhodium ammonium chloride has a high solubility, ethanol is added and then filtered to recover the rhodium ammonium chloride. Water is added to the collected precipitate, further formic acid is added and heated to 80 ° C., and rhodium ammonium chloride is reduced under a pH of about 4 to precipitate rhodium black (metal rhodium fine particles), which is filtered. Then, rhodium black is recovered.

また、ヘキサクロロロジウム酸アンモニウム水溶液にギ酸を加えて還元し、ロジウムブラックを回収し、これを還元雰囲気下で７００℃〜９００℃で焼成してロジウムスポンジを製造する方法が知られている（特開平２００７−２７０２２８号公報）。   Further, there is known a method for producing rhodium sponge by adding formic acid to an ammonium hexachlororhodate aqueous solution to reduce rhodium black and firing it at 700 ° C. to 900 ° C. in a reducing atmosphere (Japanese Patent Laid-Open No. Hei. 2007-270228).

特開平２００７−２７０２２８号公報Japanese Patent Laid-Open No. 2007-270228

上記従来技術は、次のような問題点がある。
先ず、亜硝酸ロジウムが分解される際に大量のNOx（窒素酸化物）が発生するため、作業に危険を伴う。次に、塩化ロジウムアンモニウムを回収する際に、大量のエタノールを使用するので、濾液中に含まれるエタノールによって水処理への負荷が高まり、処理コストが嵩む。 The above prior art has the following problems.
First, when rhodium nitrite is decomposed, a large amount of NOx (nitrogen oxide) is generated, which is dangerous to work. Next, since a large amount of ethanol is used when recovering rhodium ammonium chloride, the burden on water treatment increases due to the ethanol contained in the filtrate, and the treatment cost increases.

本発明は、従来技術の上記問題を解消したものであり、大量の窒素酸化物(NOx)を発生させることがなく、また、エタノールを用いないので、水処理への負荷を増大させることのない、ロジウムブラックの製造方法を提供する。   The present invention solves the above-mentioned problems of the prior art, does not generate a large amount of nitrogen oxides (NOx), and does not use ethanol, so does not increase the load on water treatment A method for producing rhodium black is provided.

本発明は、以下の構成によって上記問題を解決したロジウムブラックの製造方法に関する。
〔１〕 亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に、水およびアンモニウム塩を添加し、加熱すると共にｐＨを強酸性の範囲に調整して亜硝酸塩化ロジウムを生成させ、次いで、ギ酸を加えて亜硝酸塩化ロジウムを還元して金属ロジウム（ロジウムブラック）を生成させることを特徴とするロジウムブラックの製造方法。
〔２〕 亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に、水およびアンモニウム塩を添加した後に、６０℃〜８０℃に加熱し、塩酸を加えてｐＨ１〜２に調整する上記[１]に記載するロジウムブラックの製造方法。
〔３〕 ギ酸を添加して還元を行う際、液温を６０℃〜８０℃に加熱し、ｐＨ３〜５に調整する上記[１]または上記[２]に記載するロジウムブラックの製造方法。 The present invention relates to a method for producing rhodium black, which solves the above problems by the following constitution.
[1] To a solution of ammonium rhodium nitrite or a salt thereof, water and ammonium salt are added, heated and adjusted to a strongly acidic range to produce rhodium nitrite chloride, and then formic acid is added. A method for producing rhodium black, comprising reducing rhodium nitrite chloride to produce metal rhodium (rhodium black).
[2] In the above [1], after adding water and an ammonium salt to a solution of rhodium ammonium nitrite or a salt thereof, the mixture is heated to 60 ° C. to 80 ° C. and adjusted to pH 1-2 by adding hydrochloric acid. A method for producing rhodium black.
[3] The method for producing rhodium black according to the above [1] or [2], wherein when the formic acid is added and the reduction is performed, the liquid temperature is heated to 60 ° C. to 80 ° C. and adjusted to pH 3 to 5.

本発明の製造方法によれば、亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に塩化アンモニウム等のアンモニウム塩を添加して、亜硝酸イオンをアンモニウムイオンと反応させて分解するので、亜硝酸イオンは窒素ガスになり、従来のような大量の窒素化合物(Nox)が発生しない。   According to the production method of the present invention, an ammonium salt such as ammonium chloride is added to a rhodium nitrite ammonium solution or a salt solution thereof, and nitrite ions are reacted with ammonium ions to decompose them. It becomes a gas and a large amount of nitrogen compound (Nox) is not generated.

また、本発明の製造方法によれば、エタノールを使用しないので、水処理への負荷が小さく、処理コストを低減できるので、経済的に有利である。   Further, according to the production method of the present invention, since ethanol is not used, the load on water treatment is small and the treatment cost can be reduced, which is economically advantageous.

更に、本発明の製造方法によれば、亜硝酸ロジウムの分解工程とギ酸による還元工程を主な処理工程とし、従来の製造方法よりも処理工程が簡略であるので、ロジウムブラックを効率良く製造することができる。   Furthermore, according to the production method of the present invention, the rhodium nitrite decomposition step and the formic acid reduction step are the main treatment steps, and the treatment steps are simpler than the conventional production method, so that rhodium black is produced efficiently. be able to.

本発明の製造方法の概略を示すフローチャート。The flowchart which shows the outline of the manufacturing method of this invention. 従来の製造方法の概略を示すフローチャート。The flowchart which shows the outline of the conventional manufacturing method.

以下、本発明の実施形態を、図１を参照して具体的に説明する。
図１は本発明に係る製造方法の概略を示すフローチャートである。図示するように、本発明の製造方法は、亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に、水およびアンモニウム塩を添加し、加熱すると共にｐＨを強酸性の範囲に調整して亜硝酸塩化ロジウムを生成させ、次いで、ギ酸を加えて亜硝酸塩化ロジウムを還元して金属ロジウム（ロジウムブラック）を生成させることを特徴とするロジウムブラックの製造方法である。 Hereinafter, an embodiment of the present invention will be specifically described with reference to FIG.
FIG. 1 is a flowchart showing an outline of a manufacturing method according to the present invention. As shown in the drawing, in the production method of the present invention, rhodium nitrite chloride is added by adding water and ammonium salt to a solution of rhodium ammonium nitrite or a salt thereof, heating and adjusting the pH to a strongly acidic range. Then, rhodium nitrite chloride is reduced by adding formic acid to produce metal rhodium (rhodium black).

亜硝酸ロジウムアンモニウム溶液に水およびアンモニウム塩を添加することにより、次式[１]に示すように、亜硝酸イオンがアンモニウムイオンと反応して分解される。なお、亜硝酸ロジウムアンモニウム塩溶液、例えばＮａ塩溶液〔Na(NH4)2[Rh(NO2)6]〕を用いた場合には、Naイオンが生成する以外は次式[１]と同様の分解反応が進む。
(NH4)3[Rh(NO2)6] + ５MH4Cl → RhCl5(NO2)3- + ５N2 + １０H2O + ３NH4 +…[１] By adding water and ammonium salt to the rhodium ammonium nitrite solution, as shown in the following formula [1], nitrite ions react with ammonium ions and decompose. When a rhodium ammonium nitrite solution such as a Na salt solution [Na (NH 4 ) 2 [Rh (NO 2 ) 6 ]] is used, it is the same as the following formula [1] except that Na ions are generated. The decomposition reaction proceeds.
(NH 4 ) 3 [Rh (NO 2 ) 6 ] + 5MH 4 Cl → RhCl 5 (NO 2 ) 3- + 5N 2 + 10H 2 O + 3NH 4 + … [1]

上記亜硝酸ロジウムアンモニウムの分解は加熱下で行う。具体的には、６０℃以上が適当であり、６０℃〜８０℃が好ましい。液温が６０℃より低いと工業的に必要な反応速度が得られない。   The decomposition of rhodium ammonium nitrite is carried out under heating. Specifically, 60 ° C. or higher is appropriate, and 60 ° C. to 80 ° C. is preferable. When the liquid temperature is lower than 60 ° C., an industrially required reaction rate cannot be obtained.

亜硝酸ロジウムアンモニウムの分解反応は、溶液を強酸性に調整するのが好ましい。具体的には、溶液のｐＨを１〜２に調整すると良い。ｐＨが１未満であると、NOxが発生し易くなり、また、ｐＨが２より大きいと、工業的に必要な反応速度を得難くなる。   In the decomposition reaction of rhodium ammonium nitrite, the solution is preferably adjusted to be strongly acidic. Specifically, the pH of the solution may be adjusted to 1-2. When the pH is less than 1, NOx is likely to be generated, and when the pH is greater than 2, it is difficult to obtain an industrially required reaction rate.

亜硝酸ロジウムアンモニウム塩の分解後、ギ酸を加えることにより、次式[２]に示すように、亜硝酸塩化ロジウムがギ酸によって還元され、金属ロジウム（ロジウムブラック）が析出する。
２RhCl5(NO2) +３HCOOH +２NH4 + → ２Rh↓+５Cl- +２N2 +４H2O +６H+ +３CO2 …〔２〕 After the decomposition of the rhodium nitrite ammonium salt, formic acid is added to reduce rhodium nitrite chloride with formic acid and deposit metal rhodium (rhodium black) as shown in the following formula [2].
2RhCl 5 (NO 2 ) + 3HCOOH + 2NH 4 + → 2Rh ↓ + 5Cl − + 2N 2 + 4H 2 O + 6H + + 3CO 2 … [2]

ギ酸による還元は、反応温度６０℃〜８０℃、ｐＨ３〜５、望ましくは、ｐＨ３.５〜４.５に調整すると良い。反応温度が６０℃より低いと工業的に必要な反応速度を得難くなり、８０℃より高いと反応槽の耐久性に影響が大きく、工業的な実施が困難になる。また、ｐＨが上記範囲より低いと、微細なコロイド状のロジウムブラックが生成し、濾過回収するのが難しく、ｐＨが上記範囲より高いと、工業的に必要な反応速度を得られない。   The reduction with formic acid may be adjusted to a reaction temperature of 60 ° C. to 80 ° C., pH 3 to 5, preferably pH 3.5 to 4.5. When the reaction temperature is lower than 60 ° C, it is difficult to obtain an industrially required reaction rate. When the reaction temperature is higher than 80 ° C, the durability of the reaction vessel is greatly affected, and industrial implementation becomes difficult. On the other hand, if the pH is lower than the above range, fine colloidal rhodium black is generated and difficult to collect by filtration. If the pH is higher than the above range, an industrially required reaction rate cannot be obtained.

ギ酸の添加量は、亜硝酸塩化ロジウムに含まれるロジウム量の１２倍当量以上が好ましい。ギ酸の量が１２倍当量より少ないと亜硝酸塩化ロジウムの還元が不十分になる。上記還元処理によって析出したロジウムブラックを固液分離して回収する。   The amount of formic acid added is preferably 12 times the amount of rhodium contained in rhodium nitrite chloride. When the amount of formic acid is less than 12 times equivalent, the reduction of rhodium nitrite chloride is insufficient. The rhodium black precipitated by the reduction treatment is recovered by solid-liquid separation.

本発明の実施例を比較例と共に示す。なお、各例において、原料の亜硝酸ロジウムアンモニウムに含まれるロジウム含有量は何れも２３wt％である。   The Example of this invention is shown with a comparative example. In each example, the rhodium content contained in the raw material rhodium ammonium nitrite is 23 wt%.

〔実施例１〕
亜硝酸ロジウムアンモニウム３.２gと、水５０mlを混合し、これに塩化アンモニウム４.２gを添加した。次いで、これを加熱しながら塩酸を添加し、液温８０℃、ｐＨ１.１に調整し、３０分混合し反応させた。この反応によって亜硝酸ロジウム塩が分解し、透明な黄色い液が得られた。この間、NOxは発生しなかった。次いで、ギ酸を加え、温度８０℃、ｐＨ４に調整し、１時間混合した。ｐHはアンモニアと塩酸を逐次加えることによって制御した。その結果、液中のロジウムイオンが還元され、ロジウムブラック０.７２ｇ（乾燥重量）を得た。回収率は９７.３3%であった。 [Example 1]
3.2 g of rhodium ammonium nitrite and 50 ml of water were mixed, and 4.2 g of ammonium chloride was added thereto. Then, while heating this, hydrochloric acid was added to adjust the liquid temperature to 80 ° C. and pH 1.1, and the mixture was reacted for 30 minutes. By this reaction, rhodium nitrite was decomposed, and a transparent yellow liquid was obtained. During this time, NOx did not occur. Next, formic acid was added to adjust the temperature to 80 ° C. and pH 4, and mixed for 1 hour. The pH was controlled by sequentially adding ammonia and hydrochloric acid. As a result, rhodium ions in the liquid were reduced to obtain 0.72 g (dry weight) of rhodium black. The recovery rate was 97.3%.

〔実施例２〕
亜硝酸ロジウムアンモニウムの分解工程において、加熱温度を７０℃、ｐＨ１.８に調整した以外は実施例１と同様にしてロジウムブラックを回収した。回収率は９７.３%であった。また、亜硝酸ロジウムアンモニウムの分解工程でNOxは発生しなかった。 [Example 2]
In the decomposition process of rhodium ammonium nitrite, rhodium black was recovered in the same manner as in Example 1 except that the heating temperature was adjusted to 70 ° C. and pH 1.8. The recovery rate was 97.3%. Further, NOx was not generated during the decomposition process of rhodium ammonium nitrite.

〔実施例３〕
亜硝酸ロジウムアンモニウムの分解工程において、塩化アンモニウム添加量を６.３gとした以外は実施例１と同様にしてロジウムブラックを回収した。回収率は９８.５%であった。また、亜硝酸ロジウムアンモニウムの分解工程でNOxは発生しなかった。 Example 3
Rhodium black was recovered in the same manner as in Example 1 except that in the decomposition process of rhodium ammonium nitrite, the amount of ammonium chloride added was changed to 6.3 g. The recovery rate was 98.5%. Further, NOx was not generated during the decomposition process of rhodium ammonium nitrite.

〔比較例１〕
亜硝酸ロジウムアンモニウム３.２gと、水５０mlを混合し、加熱しながら塩酸を添加し、液温８０℃、ｐＨ１〜２に調整し、３０分混合したが、亜硝酸ロジウムアンモニウムは分解せず、透明な黄色液体に変化しなかった。塩化アンモニウムを添加しないので、亜硝酸イオンとアンモニウムイオンとの反応による亜硝酸イオンの分解が行われなかったと推察される。次いで、ギ酸を加え、温度８０℃、およびｐＨ４に調整し、１時間混合した。ｐHはアンモニアと塩酸を逐次加えることによって制御した。しかし、ロジウムブラックは生成しなかった。 [Comparative Example 1]
Mix 3.2g of rhodium ammonium nitrite and 50ml of water, add hydrochloric acid while heating, adjust to liquid temperature 80 ° C, pH 1-2, and mix for 30 minutes, but rhodium ammonium nitrite does not decompose, It did not change to a clear yellow liquid. Since ammonium chloride is not added, it is presumed that nitrite ions were not decomposed by the reaction between nitrite ions and ammonium ions. Next, formic acid was added to adjust the temperature to 80 ° C. and pH 4, and mixed for 1 hour. The pH was controlled by sequentially adding ammonia and hydrochloric acid. However, rhodium black was not produced.

〔比較例２〕
亜硝酸ロジウムアンモニウム３.２gと、水５０mlを混合し、これに塩化アンモニウム４.２gを添加した。次いで、これを加熱して液温８０℃にし、ｐＨを調整せず、３０分混合したが、亜硝酸ロジウムアンモニウムは分解せず、透明な黄色液体に変化しなかった。溶液が強酸性になるようにｐＨを調整しないので、亜硝酸イオンとアンモニウムイオンとの反応による亜硝酸イオンの分解が行われなかったと推察される。次いで、ギ酸を加え、温度８０℃、ｐＨ４に調整し、１時間混合した。ｐHはアンモニアと塩酸を逐次加えることによって制御した。しかし、ロジウムブラックは生成しなかった。 [Comparative Example 2]
3.2 g of rhodium ammonium nitrite and 50 ml of water were mixed, and 4.2 g of ammonium chloride was added thereto. Next, this was heated to reach a liquid temperature of 80 ° C., and the pH was not adjusted and mixed for 30 minutes, but rhodium ammonium nitrite did not decompose and did not change to a transparent yellow liquid. Since the pH is not adjusted so that the solution becomes strongly acidic, it is assumed that nitrite ions were not decomposed by the reaction between nitrite ions and ammonium ions. Next, formic acid was added to adjust the temperature to 80 ° C. and pH 4, and mixed for 1 hour. The pH was controlled by sequentially adding ammonia and hydrochloric acid. However, rhodium black was not produced.

〔比較例３（図２参照）〕
亜硝酸ロジウムアンモニウム３.２gに水２５ml、塩酸２５mlを混合し、８０℃に加熱して赤色の塩化ロジウム水溶液を得た。しかし、多量のNOxが発生した。放冷後、これに塩化アンモニウム５ｇを添加して混合し、塩化ロジウムアンモニウムを生成させた。このままでは塩化ロジウムアンモニウムの溶解度が大きいことから、エタノール７５mlを加えて濾過し、濾液１２５mlを分離し、塩化ロジウムアンモニウムを回収した。この回収物に水５０ml混合し、ギ酸を加え、温度８０℃、ｐＨ４に調整し、１時間混合した。ｐＨはアンモニアと塩酸を逐次加えることで制御した。その結果、乾燥量１.０gのロジウムブラックを回収した。 [Comparative Example 3 (see FIG. 2)]
25 g of water and 25 ml of hydrochloric acid were mixed with 3.2 g of rhodium ammonium nitrite and heated to 80 ° C. to obtain a red aqueous rhodium chloride solution. However, a large amount of NOx was generated. After allowing to cool, 5 g of ammonium chloride was added and mixed to produce ammonium rhodium chloride. Since the solubility of rhodium ammonium chloride is high as it is, 75 ml of ethanol was added and filtered, and 125 ml of the filtrate was separated to recover rhodium ammonium chloride. The recovered material was mixed with 50 ml of water, added with formic acid, adjusted to a temperature of 80 ° C. and a pH of 4, and mixed for 1 hour. The pH was controlled by sequentially adding ammonia and hydrochloric acid. As a result, 1.0g of rhodium black was recovered.

Claims (3)

亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に、水およびアンモニウム塩を添加し、加熱すると共にｐＨを強酸性の範囲に調整して亜硝酸塩化ロジウムを生成させ、次いで、ギ酸を加えて亜硝酸塩化ロジウムを還元して金属ロジウム（ロジウムブラック）を生成させることを特徴とするロジウムブラックの製造方法。
To a solution of rhodium ammonium nitrite or a salt thereof, water and ammonium salt are added, heated and the pH is adjusted to a strongly acidic range to form rhodium nitrite chloride, and then formic acid is added to nitrite chloride. A method for producing rhodium black, comprising reducing rhodium to produce rhodium (rhodium black).
亜硝酸ロジウムアンモニウム溶液またはその塩の溶液に、水およびアンモニウム塩を添加した後に、６０℃〜８０℃に加熱し、塩酸を加えてｐＨ１〜２に調整する請求項１に記載するロジウムブラックの製造方法。
2. The production of rhodium black according to claim 1, wherein water and an ammonium salt are added to a solution of rhodium ammonium nitrite or a salt thereof, and then heated to 60 ° C. to 80 ° C. and adjusted to pH 1 to 2 by adding hydrochloric acid. Method.
ギ酸を添加して還元を行う際、液温を６０℃〜８０℃に加熱し、ｐＨ３〜５に調整する請求項１または請求項２に記載するロジウムブラックの製造方法。 The method for producing rhodium black according to claim 1 or 2, wherein when the formic acid is added for reduction, the liquid temperature is heated to 60 ° C to 80 ° C and adjusted to pH 3-5.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011094198A (en) * 2009-10-30 2011-05-12 Mitsubishi Materials Corp Rhodium reduction method
CN114178540A (en) * 2021-10-18 2022-03-15 英特派铂业股份有限公司 Rapid and low-loss reduction method of potassium hexanitrosorhodate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011094198A (en) * 2009-10-30 2011-05-12 Mitsubishi Materials Corp Rhodium reduction method
CN114178540A (en) * 2021-10-18 2022-03-15 英特派铂业股份有限公司 Rapid and low-loss reduction method of potassium hexanitrosorhodate
CN114178540B (en) * 2021-10-18 2023-09-15 英特派铂业股份有限公司 Quick and low-loss reduction method of potassium hexanitrosorhodium

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