CN102070210A - Synthesis method of halogen ion-free rhodium nitrate - Google Patents
Synthesis method of halogen ion-free rhodium nitrate Download PDFInfo
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- CN102070210A CN102070210A CN 201010580005 CN201010580005A CN102070210A CN 102070210 A CN102070210 A CN 102070210A CN 201010580005 CN201010580005 CN 201010580005 CN 201010580005 A CN201010580005 A CN 201010580005A CN 102070210 A CN102070210 A CN 102070210A
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Abstract
The invention provides a preparation method of halogen ion-free rhodium nitrate. The preparation method is as follows: adding concentrated nitric acid in rhodium iodate which is directly used as raw material to react and obtain rhodium nitrate; adding hydrogen peroxide to remove excess the iodine ions in the solution; carrying out vacuum filtration; and preparing halogen ion-free rhodium nitrate with a water bath. The specific steps are as follows: in the rhodium iodate raw material, adding 65% concentrated nitric acid which is 4-20 times of rhodium iodate by mole, carrying out a reflux reaction for 1-4 hours at 60-110 DEG C to obtain rhodium nitrate; adding 30% hydrogen peroxide which is 0.4-5 times of rhodium iodate by mole, reacting for 1-3 hours to remove excess iodine ions in the solution; and finally, obtaining halogen ion-free rhodium nitrate with a 80-95 DEG C of water bath. The preparation method has the following characteristics: 1) the solubility of rhodium iodate is lower in water relative to rhodium hydroxide, rhodium iodate is easier to clean and has low loss; 2) the process is easy to perform quantitatively, so that the quality of the product can be controlled; 3) the reaction operation is convenient, the large-scale production of rhodium iodate is realized, rhodium iodate is easy to obtain; and 4) the reaction posttreatment is simple, vacuum filtration and evaporation in the water bath are just needed, and the purity of the product is high.
Description
Technical field
What the present invention relates to is a kind of synthetic method of halogen ion rhodium nitrate.
Background technology
Vehicle exhaust is one of main source of topsoil.The motor vehicle exhaust rules of developed country are strict day by day in the world, and following automobile must reach low emission, minimum discharge, even the requirement of zero release.The catalytic cleaning of car tail gas technology is proved to be one of method of the most effective control vehicle emission pollution.Catalytic cleaner arises at the historic moment, and this device is positioned in the exhaust system of automobile, and its effect is to reduce most of exhaust emission that engine is discharged; Triple mode catalytic converter is by a metal shell, a net bottom frame and a Catalytic Layer (containing precious metals such as platinum, rhodium) are formed, can remove 90% (so-called ternary is meant the chemical reaction that is taken place when removing toward these three kinds of compounds) of HC (hydrocarbon polymer), CO (carbon monoxide) and three kinds of principal pollutant matter of NOx (oxynitrides), when waste gas process cleaner, platinum catalyst will impel HC and born water vapor of CO oxidation and carbonic acid gas; Rhodium catalyst can impel NOx to be reduced to nitrogen and oxygen.And rhodium nitrate is a kind of common rhodium soluble compound, and 72% is used for preparing the automobile three-way catalyst, and 15% is used for being used as the precursor of homogeneous catalyst and heterogeneous catalyst, and remaining is directly as catalyzer.
Halide-ions has strict requirement in the rhodium nitrate, can make that not so its catalytic performance and stability reduce greatly, even cause poisoning of catalyst, and therefore preparing halogen ion rhodium nitrate has very large necessity; The preparation method who describes on the known references has two kinds at present:
The one, utilize sodium pyrosulfate dissolving rhodium powder, then gained solution is added alkali, obtain rhodium hydroxide, the ionized water of entering washs, and adds concentrated nitric acid at last and prepares; Its shortcoming is that rhodium hydroxide has certain solubility in water, can cause bigger loss, and the quantitatively control of having no idea in the time of dissolved.
The 2nd, utilize iodate rhodium adding concentrated nitric acid to boil and obtain rhodium nitrate, then at the 105-110 ℃ of dry residue nitric acid of removing, yet can partly be decomposed into rhodium oxide except that rhodium nitrate in the nitre process in drying.
Summary of the invention
The objective of the invention is to overcome the weakness that exists in the existing traditional processing technology, and a kind of preparation method of halogen ion rhodium nitrate is provided.
The objective of the invention is to finish by following technical solution, described preparation method is: directly adopting the iodate rhodium is raw material, add concentrated nitric acid, reaction obtains rhodium nitrate, add iodide ion excessive in the hydrogen peroxide removal solution at last, last suction filtration utilizes water-bath to prepare halogen ion rhodium nitrate.
In the described iodate rhodium raw material, 4-20 times of adding iodate rhodium mole number, concentration are 65% concentrated nitric acid, after 60-110 ℃ of following back flow reaction 1-4 hour, obtain rhodium nitrate, the 0.4-5 that adds iodate rhodium mole number more doubly, concentration is 30% hydrogen peroxide, excessive iodide ion through reaction was removed in the solution in 1-3 hour utilizes 80-95 ℃ of water-bath to prepare halogen ion rhodium nitrate at last.
Described preferred version is: in iodate rhodium raw material, 10 times of adding iodate rhodium mole numbers, concentration are 65% concentrated nitric acid, obtain rhodium nitrate 90 ℃ of following back flow reaction after 2 hours, add 3 times of iodate rhodium mole number, concentration again and be 30% hydrogen peroxide, through reacting the excessive iodide ion of removing in the solution in 2 hours, utilize 90 ℃ of water-baths to prepare halogen ion rhodium nitrate at last, its reaction formula is:
2RHI3+8HNO3---------2Rh(NO3)3+3I2+2NO+4H2O
Advantage of the present invention is:
1) the relative rhodium hydroxide of iodate rhodium solubleness in water is little, and the easier washing of iodate rhodium, and loss is little;
2) process is easy to quantitatively carry out, and makes that product quality can be controlled;
3) operation is easy, and the large-scale production of iodate rhodium is easy to get;
4) post-reaction treatment is simple, only needs suction filtration, water bath method, degree of purity of production height.
Embodiment
Below with specific examples technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Preparation method of the present invention is: directly adopting the iodate rhodium is raw material, adds concentrated nitric acid, and reaction obtains rhodium nitrate, adds iodide ion excessive in the hydrogen peroxide removal solution at last, and last suction filtration utilizes water-bath to prepare halogen ion rhodium nitrate.
In the described iodate rhodium raw material, 4-20 times of adding iodate rhodium mole number, concentration are 65% concentrated nitric acid, after 60-110 ℃ of following back flow reaction 1-4 hour, obtain rhodium nitrate, the 0.4-5 that adds iodate rhodium mole number more doubly, concentration is 30% hydrogen peroxide, excessive iodide ion through reaction was removed in the solution in 1-3 hour utilizes 80-95 ℃ of water-bath to prepare halogen ion rhodium nitrate at last.
Described optimal technical scheme is: in iodate rhodium raw material, 10 times of adding iodate rhodium mole numbers, concentration are 65% concentrated nitric acid, obtain rhodium nitrate 90 ℃ of following back flow reaction after 2 hours, add 3 times of iodate rhodium mole number, concentration again and be 30% hydrogen peroxide, through reacting the excessive iodide ion of removing in the solution in 2 hours, utilize 90 ℃ of water-baths to prepare halogen ion rhodium nitrate at last.Its reaction formula is:
2RHI3+8HNO3---------2Rh(NO3)3+3I2+2NO+4H2O
After other optional technical scheme of the present invention can be selected in the data area that above-mentioned preparation method put down in writing, obtain easily after above-mentioned preferred version replaced, and these specific embodiments are not limited among following several embodiment.
Embodiment 1: in 1 L flask of mechanical stirrer and reflux condensing tube is housed, add the iodate rhodium of 65% concentrated nitric acid 200mL and 100.00 g 20.0% earlier, be heated to 90 ℃, reacted 2 hours, add 30% superoxol 10mL again, reacted 1 hour.Reaction solution sand core funnel suction filtration, gained filtrate obtains rhodium nitrate 66.10 g with 90 ℃ of water bath methods, and content is 30.0% after testing, and yield is 99.1%, and halogen ion concentration is less than 50 ppm.
Embodiment 2: reactions steps is with embodiment 1, and different is that temperature of reaction is 100 ℃, obtains rhodium nitrate 65.23 g, and content is 30.2% after testing, and yield is 98.5%, and halogen ion concentration is less than 50 ppm.
Embodiment 3: reactions steps is with embodiment 1, and enriching nitric acid reaction 1 hour obtains rhodium nitrate 62.55 g, and content is 29.8% after testing, and yield is 93.2%, and halogen ion concentration is less than 50 ppm.
Embodiment 4: reactions steps added hydroperoxidation 2 hours with embodiment 1, obtained rhodium nitrate 65.98 g, and content is 30.1% after testing, and yield is 99.3%, and halogen ion concentration is less than 50 ppm.
Embodiment 5: reactions steps is with embodiment 1, and different is not add superoxol, obtains rhodium nitrate 64.50 g, and content is 29.5% after testing, and yield is 95.1%, and halogen ion concentration is 2500ppm.
Claims (3)
1. the preparation method of a halogen ion rhodium nitrate, this method is: directly adopting the iodate rhodium is raw material, adds concentrated nitric acid, reaction obtains rhodium nitrate, add iodide ion excessive in the hydrogen peroxide removal solution at last, last suction filtration utilizes water-bath to prepare halogen ion rhodium nitrate.
2. the preparation method of halogen ion rhodium nitrate according to claim 1, it is characterized in that in the described iodate rhodium raw material, 4-20 times of adding iodate rhodium mole number, concentration are 65% concentrated nitric acid, after 60-110 ℃ of following back flow reaction 1-4 hour, obtain rhodium nitrate, the 0.4-5 that adds iodate rhodium mole number more doubly, concentration is 30% hydrogen peroxide, excessive iodide ion through reaction was removed in the solution in 1-3 hour utilizes 80-95 ℃ of water-bath to prepare halogen ion rhodium nitrate at last.
3. the preparation method of halogen ion rhodium nitrate according to claim 2, it is characterized in that, in iodate rhodium raw material, 10 times of adding iodate rhodium mole numbers, concentration are 65% concentrated nitric acid, obtain rhodium nitrate 90 ℃ of following back flow reaction after 2 hours, add 3 times of iodate rhodium mole number, concentration again and be 30% hydrogen peroxide,, utilize 90 ℃ of water-baths to prepare halogen ion rhodium nitrate at last through reacting the excessive iodide ion of removing in the solution in 2 hours.
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| CN 201010580005 CN102070210A (en) | 2010-12-09 | 2010-12-09 | Synthesis method of halogen ion-free rhodium nitrate |
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| CN 201010580005 CN102070210A (en) | 2010-12-09 | 2010-12-09 | Synthesis method of halogen ion-free rhodium nitrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264100A (en) * | 2018-03-18 | 2018-07-10 | 中船重工黄冈贵金属有限公司 | A kind of high-efficiency synthesis method of rhodium nitrate solution |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983372A (en) * | 1990-07-20 | 1991-01-08 | Brienza Walter C | Process for preparing halide-free rhodium nitrate |
| RU2208586C2 (en) * | 2000-12-19 | 2003-07-20 | Московская государственная академия тонкой химической технологии им. М.В. Ломоносова | Rhodium nitrate solution preparation method |
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2010
- 2010-12-09 CN CN 201010580005 patent/CN102070210A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983372A (en) * | 1990-07-20 | 1991-01-08 | Brienza Walter C | Process for preparing halide-free rhodium nitrate |
| RU2208586C2 (en) * | 2000-12-19 | 2003-07-20 | Московская государственная академия тонкой химической технологии им. М.В. Ломоносова | Rhodium nitrate solution preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264100A (en) * | 2018-03-18 | 2018-07-10 | 中船重工黄冈贵金属有限公司 | A kind of high-efficiency synthesis method of rhodium nitrate solution |
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Application publication date: 20110525 |