CN106854001A - 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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- CN106854001A CN106854001A CN201611176364.0A CN201611176364A CN106854001A CN 106854001 A CN106854001 A CN 106854001A CN 201611176364 A CN201611176364 A CN 201611176364A CN 106854001 A CN106854001 A CN 106854001A
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- reducing agent
- iridium
- chloride
- iridous chloride
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of control reducing preparation method of iridous chloride, belong to reduction technique field.Tetravalence iridium chloride and reducing agent are added in there-necked flask according to a certain percentage, under the conditions of magnetic agitation, tetravalence iridium is all converted to trivalent during constant temperature is restored to solution, and condensation reflux unit is used in course of reaction, reduce the volatilization of reducing agent, control reaction system stabilization.The method is simple 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 field, 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, and iridium catalyst is contained frequently as synthesizing other iridic compounds and preparing
Initial feed.It is widely used in petrochemical industry and organic synthesis, hydrogenation catalyst, polymerization catalyst containing iridic compound and catalyst
Deng field.For example, basic material of the hydrated iridium trichloride as synthesis complex of iridium, plays important to the development of phosphor material
Effect.
The fusing point of iridium is (2440 DEG C) very high, remains to keep low oxygen permeability at 2100 DEG C, at 2280 DEG C not with carbon
React, and can effectively prevent Carbon diffusion, be a kind of most promising ORC material；And iridium corrosion resistant 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, and reason is that iridous chloride is more easy to be oxidized, and the iridium film formed in electrode surface is more caused
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, 600 DEG C is heated to or is shone 15min with the bright light of direct sunshine or red-hot magnesium rod
Left and right, obtains pure IrCl3, but the IrCl that the method is obtained3Water insoluble, sour, alkali, inconvenient extensive use in the industry.
The content of the invention
For the deficiency of existing iridous chloride preparation method, the control the invention provides a kind of iridous chloride reduces preparation
Method, it is characterised 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 there-necked flask, under the conditions of magnetic agitation, constant temperature reductase 12~10 hour, tetravalence iridium is all converted to trivalent into solution, so
Iridium content is 2mol/L during the trivalent iridium solution that will be obtained afterwards carries out being concentrated into solution, 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 up of acids reducing agent, alcohols reducing agent and hydrazine reducing agent.
The acids reducing agent is the one kind in ascorbic acid, acetic acid, accounts for the 50~75% of reducing agent gross mass；The alcohol
Class reducing agent be methyl alcohol, propyl alcohol, polyethylene glycol in one or more, the 15~30% of reducing agent gross mass are accounted for altogether；Institute
Hydrazine reducing agent is stated for hydrazine hydrochloride, hydrazine hydrate, one or more in hydrazine sulfate, account for altogether reducing agent gross mass 10~
20%.
Described reduction temperature is 75~100 DEG C.
Condensation reflux unit is installed on described there-necked flask, the volatilization of reducing agent is reduced, it is ensured that the stabilization of system.
The advantage of the invention is that：
(1) course of reaction can remove the addition of reagent invariably, it is to avoid the introducing of other metal impurities, product purity is high；
(2) reduction reaction is controlled to enter by the liquid volume for controlling the addition and condensation reflux unit of reducing agent to flow back
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 is reduced completely
It is trivalent.
Brief 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 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：To 100 grams of chloro-iridic acid of addition, reducing agent propyl alcohol in the there-necked flask being placed in water bath with thermostatic control equipment
2g, hydrazine hydrochloride 1.5g, ascorbic acid 6.5g, the temperature in control water bath with thermostatic control equipment open magnetic agitation system at 75~100 DEG C
System, carries out constant temperature stirring, and constant temperature is reduced 3 hours and is all converted to trivalent to tetravalence iridium in solution；
2nd step, concentration：The trivalent iridium aqueous solution that will be obtained is concentrated, and distills out excessive water, obtains the concentration of trivalent iridium
Liquid, iridium content is 2mol/L in the 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%.
Iridous chloride to obtaining has carried out X-ray photoelectron spectroscopic analysis, and its result is as shown in figure 1, can be with from figure
See the spectral peak of Ir, Cl, O, C, wherein Cl elements are more obvious with the spectral peak of Ir elements, the 4f7/2 characteristic spectral lines of Ir, in sample
The combination of Ir can be 62.78ev, and iridium is with Ir in showing sample3+Form exist, meet iridium from raw material+4 valencys reduction
To the process of+trivalent.Because the photoelectron intensity that sample surfaces certain atoms is projected is and the content of the element in sample into line
Sexual intercourse, therefore the ratio between content of chlorine element and iridium knowable to semi-quantitative analysis is carried out to constituent content using XPS (Fig. 2)
It is 3:1, it is believed that elemental indium is with Ir in this kind of compound3+Form is present.
Claims (6)
1. the control reducing preparation method of a kind of iridous chloride, it is characterised in that by tetravalence iridium chloride and reducing agent according to
Certainty ratio is added in the there-necked flask being placed in water bath with thermostatic control equipment, and under the conditions of magnetic agitation, constant temperature reductase 12~10 are small
When, iridium content is 2mol/L during the trivalent iridium solution that then will be obtained carries out being concentrated into solution, finally by concentrate solution at 90 DEG C
Under crystallized, obtain iridous chloride crystal.
2. the method that prepared by a kind of iridous chloride as claimed in claim 1, it is characterised in that tetravalence iridium chloride and reducing agent
Mass ratio is 10:1.
3. the control reducing preparation method of a kind of iridous chloride as claimed in claim 1, it is characterised in that the reducing agent by
Acids reducing agent, alcohols reducing agent and hydrazine reducing agent composition.
4. a kind of control reducing preparation method of iridous chloride as claimed in claim 3, it is characterised in that the acids reduction
Agent is the one kind in ascorbic acid, acetic acid, accounts for the 50~75% of reducing agent gross mass；The alcohols reducing agent be methyl alcohol, propyl alcohol,
One or more in polyethylene glycol, account for the 15~30% of reducing agent gross mass altogether；The hydrazine reducing agent be hydrazine hydrochloride,
Hydrazine hydrate, one or more in hydrazine sulfate account for the 10~20% of reducing agent gross mass altogether.
5. a kind of control reducing preparation method of iridous chloride as claimed in claim 1, it is characterised in that described reduction temperature
Degree is 75~100 DEG C.
6. a kind of preparation method of iridous chloride as claimed in claim 1, it is characterised in that installed on described there-necked flask
Condensation reflux unit, reduces the volatilization of reducing agent, control reaction system stabilization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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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 CN106854001B (en) | 2018-06-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110937989A (en) * | 2018-09-21 | 2020-03-31 | 中国石油化工股份有限公司 | Synthesis method of acetic acid |
| CN110937992A (en) * | 2018-09-21 | 2020-03-31 | 中国石油化工股份有限公司 | Preparation method of iridium acetate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06298535A (en) * | 1993-04-09 | 1994-10-25 | Tanaka Kikinzoku Kogyo Kk | Production of chloropentaammine iridium dichloride crystal |
| US20080248195A1 (en) * | 2004-03-31 | 2008-10-09 | Studiengesellschaft Kohle Mbh | Method for the Production of Iridium Oxide Coatings |
| 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 |
-
2016
- 2016-12-19 CN CN201611176364.0A patent/CN106854001B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06298535A (en) * | 1993-04-09 | 1994-10-25 | Tanaka Kikinzoku Kogyo Kk | Production of chloropentaammine iridium dichloride crystal |
| US20080248195A1 (en) * | 2004-03-31 | 2008-10-09 | Studiengesellschaft Kohle Mbh | Method for the Production of Iridium Oxide Coatings |
| 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 (2)
| Title |
|---|
| 刘时杰: "《铂族金属冶金学》", 30 June 2013 * |
| 徐光: ""铱基配合物的合成及其工艺研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110937989A (en) * | 2018-09-21 | 2020-03-31 | 中国石油化工股份有限公司 | Synthesis method of acetic acid |
| CN110937992A (en) * | 2018-09-21 | 2020-03-31 | 中国石油化工股份有限公司 | Preparation method of iridium acetate |
| 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 |
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| CN106854001B (en) | 2018-06-19 |
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