CN106854001B - A kind of control reducing preparation method of iridous chloride - Google Patents
A kind of control reducing preparation method of iridous chloride Download PDFInfo
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- CN106854001B CN106854001B CN201611176364.0A CN201611176364A CN106854001B CN 106854001 B CN106854001 B CN 106854001B CN 201611176364 A CN201611176364 A CN 201611176364A CN 106854001 B CN106854001 B CN 106854001B
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- reducing agent
- iridium
- chloride
- iridous chloride
- hydrazine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/005—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of control reducing preparation methods of iridous chloride, belong to reduction technique field.Tetravalence iridium chloride and reducing agent are added in three-necked flask according to a certain percentage, under the conditions of magnetic agitation, constant temperature is restored to tetravalence iridium in solution and is all converted to trivalent, and condensation reflux unit is used in reaction process, the volatilization of reducing agent is reduced, control reaction system is stablized.This method is easy to operate, and flow is short, and reduction process is fully controllable, stable content, it is ensured that tetravalence iridium is reduced to trivalent completely, and the iridous chloride product purity of preparation is high.
Description
Technical field
The invention belongs to reduction technique fields, and in particular to a kind of control reducing preparation method of iridous chloride.
Background technology
The chloride of iridium is the common compound of iridium, frequently as the other iridic compounds of synthesis and is prepared containing iridium catalyst
Initial feed.It is widely used in petrochemical industry and organic synthesis, hydrogenation catalyst, polymerization catalyst containing iridic compound and catalyst
The fields of grade.For example, basic material of the hydrated iridium trichloride as synthesis complex of iridium, plays the development of phosphor material important
Effect.
The fusing point of iridium is very high (2440 DEG C), remains to keep low oxygen permeability at 2100 DEG C, at 2280 DEG C not with carbon
It reacts, and can effectively prevent Carbon diffusion, be a kind of most promising antioxidant coating material；And the corrosion resistant of iridium at high temperature
Erosion and antioxygenic property are excellent, the environment of high temperature corrosion-resisting are required for some frequently as protection film layer, as turbogenerator
Thermal structure surface has a wide range of applications in high-tech sectors such as Aeronautics and Astronautics, navigations.Industrially begin to use three at present
Iridium chloride cooks electroplate liquid instead of chloro-iridic acid, the reason is that iridous chloride is more easy to be aoxidized, is more caused in the iridium film that electrode surface is formed
It is close.
Traditional method for preparing iridous chloride is by powder iridium or Ir (OH)4Be placed in quartz ampoule, be passed through it is not oxygen-containing but
The chlorine of a small amount of carbon monoxide is mixed with, be heated to 600 DEG C or shines 15min with the bright light of direct sunlight or red-hot magnesium rod
Left and right, obtains pure IrCl3, but the IrCl that the method obtains3Not soluble in water, sour, alkali, inconvenient extensive use in the industry.
Invention content
For the deficiency of existing iridous chloride preparation method, the control the present invention provides a kind of iridous chloride restores preparation
Method, which is characterized in that tetravalence iridium chloride and reducing agent are added to according to a certain percentage and are placed in water bath with thermostatic control equipment
In three-necked flask, under the conditions of magnetic agitation, constant temperature reductase 12~10 hour, until tetravalence iridium is all converted to trivalent in solution, so
It is 2mol/L be concentrated into iridium content in solution by obtained trivalent iridium solution afterwards, and last concentrate solution is tied at 90 DEG C
Crystalline substance obtains iridous chloride crystal.
Wherein, tetravalence iridium chloride and reducing agent mass ratio are 10:1.
The reducing agent is made of acids reducing agent, alcohols reducing agent and hydrazine reducing agent.
The acids reducing agent is ascorbic acid, one kind in acetic acid, accounts for the 50~75% of reducing agent gross mass；The alcohol
Class reducing agent is methanol, the one or more in propyl alcohol, polyethylene glycol, accounts for the 15~30% of reducing agent gross mass altogether；Institute
Hydrazine reducing agent is stated as hydrazine hydrochloride, hydrazine hydrate, the one or more in hydrazine sulfate, account for altogether reducing agent gross mass 10~
20%.
The reduction temperature is 75~100 DEG C.
Condensation reflux unit is installed on the three-necked flask, reduces the volatilization of reducing agent, it is ensured that the stabilization of system.
The advantage of the invention is that：
(1) reaction process can remove the addition of reagent invariably, avoid the introducing of other metal impurities, and product purity is high；
(2) by control reducing agent addition and condensation reflux unit flow back liquid volume come control reduction reaction into
Capable degree, it is possible to reduce the volatilization of solvent and reducing agent keeps the stabilization of reduction system；
(3) method is simple, and flow is short, and reduction process is fully controllable, and stable content is controllable, it is ensured that tetravalence iridium restores completely
For trivalent.
Description of the drawings
Fig. 1 is the survey scan figure of hydrated iridium trichloride；
Fig. 2 is the XPS spectrum figure of hydrated iridium trichloride.
Specific embodiment
The present invention provides a kind of control reducing preparation method of iridous chloride, with reference to the accompanying drawings and examples to this hair
It is bright to be described further.
The operating procedure that chloro-iridic acid is reduced to iridous chloride is as follows：
1st step, reduction：100 grams of chloro-iridic acid, reducing agent propyl alcohol are added in into the three-necked flask being placed in water bath with thermostatic control equipment
2g, hydrazine hydrochloride 1.5g, ascorbic acid 6.5g control the temperature in water bath with thermostatic control equipment to open magnetic agitation system at 75~100 DEG C
System, carries out constant temperature stirring, and constant temperature restores 3 hours and is all converted to trivalent to tetravalence iridium in solution；
2nd step, concentration：Obtained trivalent iridium aqueous solution is concentrated, distills out excessive water, obtains the concentration of trivalent iridium
Liquid, iridium content is 2mol/L in iridous chloride aqueous solution after concentration；
3rd step, crystallization：Trivalent iridium solution after concentration is placed in crystallising dish, is crystallized at 90 DEG C, crystallization time
2 hours, obtain iridous chloride crystallization 62.5g, yield rate 97.16%, iridium content 54.4%.
X-ray photoelectron spectroscopic analysis is carried out to obtained iridous chloride, the results are shown in Figure 1, can be with from figure
See the spectral peak of Ir, Cl, O, C, wherein Cl elements and the spectral peak of Ir elements is more apparent, the 4f7/2 characteristic spectral lines of Ir, in sample
The combination of Ir can be 62.78ev, show that iridium is with Ir in sample3+Form existing for, meet iridium from raw material+4 valencys reduction
To the process of+trivalent.Since the photoelectron intensity that sample surfaces certain atoms projects is into line with the content of the element in sample
Sexual intercourse, therefore semi-quantitative analysis is carried out to constituent content using XPS (Fig. 2) and understands the ratio between chlorine element and the content of iridium
It is 3:1, it is believed that elemental indium is with Ir in such compound3+Form exists.
Claims (4)
1. the control reducing preparation method of a kind of iridous chloride, which is characterized in that by tetravalence iridium chloride and reducing agent according to one
Certainty ratio, which is added to, to be placed in the three-necked flask in water bath with thermostatic control equipment, and under the conditions of magnetic agitation, constant temperature reductase 12~10 are small
When, it is 2mol/L be then concentrated into iridium content in solution by obtained trivalent iridium solution, finally by concentrate solution at 90 DEG C
Under crystallized, obtain iridous chloride crystal；
The reducing agent is made of acids reducing agent, alcohols reducing agent and hydrazine reducing agent；
The acids reducing agent is ascorbic acid, one kind in acetic acid, accounts for the 50~75% of reducing agent gross mass；The alcohols is also
Former agent is methanol, the one or more in propyl alcohol, polyethylene glycol, accounts for the 15~30% of reducing agent gross mass altogether；The hydrazine
Class reducing agent is hydrazine hydrochloride, hydrazine hydrate, and the one or more in hydrazine sulfate account for the 10~20% of reducing agent gross mass altogether.
2. method prepared by a kind of iridous chloride as described in claim 1, which is characterized in that tetravalence iridium chloride and reducing agent
Mass ratio is 10:1.
A kind of 3. control reducing preparation method of iridous chloride as described in claim 1, which is characterized in that the reduction temperature
Degree is 75~100 DEG C.
4. a kind of preparation method of iridous chloride as described in claim 1, which is characterized in that installed on the three-necked flask
Condensation reflux unit, reduces the volatilization of reducing agent, and control reaction system is stablized.
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| CN201611176364.0A CN106854001B (en) | 2016-12-19 | 2016-12-19 | A kind of control reducing preparation method of iridous chloride |
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| CN201611176364.0A CN106854001B (en) | 2016-12-19 | 2016-12-19 | A kind of control reducing preparation method of iridous chloride |
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| CN106854001B true CN106854001B (en) | 2018-06-19 |
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| CN110937989B (en) * | 2018-09-21 | 2022-09-20 | 中国石油化工股份有限公司 | Synthesis method of acetic acid |
| CN110937992B (en) * | 2018-09-21 | 2022-10-21 | 中国石油化工股份有限公司 | Preparation method of iridium acetate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408135A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Method for preparing iridous chloride hydrate |
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| JP2983123B2 (en) * | 1993-04-09 | 1999-11-29 | 田中貴金属工業株式会社 | Method for producing chloropentaammineiridium dichloride crystal |
| DE102004015633A1 (en) * | 2004-03-31 | 2005-10-20 | Studiengesellschaft Kohle Mbh | Process for the preparation of coatings of iridium oxides |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408135A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Method for preparing iridous chloride hydrate |
Non-Patent Citations (1)
| Title |
|---|
| "铱基配合物的合成及其工艺研究";徐光;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20150115;第35-40页 * |
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