CN106810440A - A kind of preparation method of acetic acid iridium - Google Patents
A kind of preparation method of acetic acid iridium Download PDFInfo
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- CN106810440A CN106810440A CN201510845709.6A CN201510845709A CN106810440A CN 106810440 A CN106810440 A CN 106810440A CN 201510845709 A CN201510845709 A CN 201510845709A CN 106810440 A CN106810440 A CN 106810440A
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- C07C51/41—Preparation of salts of carboxylic acids
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Abstract
The present invention provides a kind of preparation method of acetic acid iridium, the described method comprises the following steps：I) iridium powder and mixed alkali are mixed and heated and are reacted；Ii washed after the product cooling for) obtaining step i) in water, stirred, separation of solid and liquid；Iii) by step ii) in separation of solid and liquid produce solid add chloroazotic acid in, heat and stir and reacted；Iv) by step iii) reaction mass cool down and carry out separation of solid and liquid, then liquid distillation and concentration is obtained into chloro-iridic acid product v) by step iv) obtain chloro-iridic acid product be added to the water, alkalescence is titrated to alkali hydroxide soln, precipitation is produced；Vi) the precipitate and separate for producing step v), and add aqueous acetic acid, heating reflux reaction；And vii) by step vi) reaction mass distillation and concentration, obtain acetic acid iridium.The method building-up process for providing of the invention is simple, iridium powder conversion per pass is high, target product yield is high, and the loss late of iridium is low.
Description
Technical field
The present invention relates to the synthesis technical field of chemical products, and in particular to a kind of preparation method of acetic acid iridium.
Background technology
Iridium is a kind of silvery white noble metal with suitable ductility, 2410 DEG C of its fusing point, 4130 DEG C of boiling point,
Generally face-centered cubic crystal.Generally, the form of commodity iridium is powdered, i.e. iridium powder.At present, the state of iridium powder
The interior market price is in 10~200,000 yuan/kilogram.
Metal iridium is to synthesize other containing iridic compound and prepare the initial feed containing iridium catalyst.Iridium and iridic compound
Extensive use be exactly that used as various chemical reactions, such as isomerization reaction, hydroformylation reaction or carbonylation are anti-
The purposes of the catalyst answered.At present, weight has been obtained by the special carbonylation of iridium or its compound for catalysis
Depending on.One of example is exactly the methanol carbonylation for generating acetic acid or the iridium catalysis of its reactive derivatives.
Acetic acid iridium is important chemical catalyst, and the catalyst of the reaction of acetic acid can be prepared as methanol carbonyl.
The traditional preparation methods of acetic acid iridium catalyst are：Metal iridium powder and basic anhydride are anti-in high temperature furnace
Should, product is dissolved in acid, and unreacted iridium powder is isolated through filtration washing, and gained filtrate is anti-with chloroazotic acid
Ying Houzai obtains ammonium chloroiridate precipitation with ammonium chloride reaction, and the ammonium chloroiridate obtained after filtration washing is anti-with chloroazotic acid again
Chloro-iridic acid should be concentrated to give；Then again with chloro-iridic acid as reaction raw materials, prepare acetic acid iridium by series reaction and urge
Agent.Not only process is complicated for this acetic acid iridium preparation technology, and the loss of iridium is larger.
The content of the invention
For defect present in prior art, it is an object of the invention to provide one kind with iridium powder as raw material, system
For process simply, the method for the few synthesis acetic acid iridium of the loss amount of iridium.
According to the present invention, there is provided a kind of method for preparing acetic acid iridium, the described method comprises the following steps：
I) iridium powder and mixed alkali are mixed and heated and are reacted；
Ii washed after the product cooling for) obtaining step i) in water, stirred, separation of solid and liquid；
Iii) by step ii) in separation of solid and liquid produce solid add chloroazotic acid in, heat and stir and reacted；
Iv) by step iii) reaction mass cool down and carry out separation of solid and liquid, then liquid distillation and concentration is obtained
Chloro-iridic acid product (in the methods of the invention as intermediate product)；
V) by step iv) obtain chloro-iridic acid product be added to the water, be titrated to alkali hydroxide soln
Alkalescence, produces precipitation；
Vi) the precipitate and separate for producing step v), and add aqueous acetic acid, heating reflux reaction；With
And
Vii) by step vi) reaction mass distillation and concentration, obtain acetic acid iridium.
The preparation method of the acetic acid iridium that the present invention is provided includes the preparation process of chloro-iridic acid, with chlorine in the prior art
The preparation process of iridium acid is compared, and the method that the present invention is provided using acid solution after step i) without dissolving reaction
Product, and directly washed using water, produce chloro-iridic acid with chloroazotic acid reaction afterwards；Thus without utilizing chlorination
Ammonium reaction is obtained after ammonium chloroiridate, just produces chloro-iridic acid with chloroazotic acid reaction again.It can be seen that, what the present invention was provided
Method is substantially simpler than existing method, and saves reagent, reduces the generation of waste liquid.Additionally, the contracting of method and step
Subtracting can bring significant advantage for noble metal reaction, because the reduction of step can reduce noble metal
Number of dropouts, so as to increase operation rate and the rate of recovery, reduction loss late, so can be cost-effective.
In the method for the invention, the water for being used preferably deionized water, distilled water or ultra-pure water.
According to the present invention, " the mixed alkali " refers to the mixture of alkali compounds, preferably alkali metal hydroxide
The solid mixture of thing and alkali-metal peroxide.
Preferably, the alkali metal hydroxide and the mass ratio of the alkali-metal peroxide are 1:(1-5),
It is preferred that 1:(2-4), further preferably 1：(2.5-3.5).According to the present invention, in the proportion, can make
Carry out the reacting quality of step i), and then active influence is brought to follow-up reaction and treatment, finally obtain
Obtain preferably reaction effect.
It is further preferred that the alkali metal hydroxide is included or selected from NaOH, potassium hydroxide and hydrogen-oxygen
Change at least one in lithium, preferably NaOH；The alkali-metal peroxide include or selected from sodium peroxide,
At least one in potassium peroxide and lithium peroxide, preferably sodium peroxide.
Certain preferred embodiments of the invention, in step i), the quality of the iridium powder is mixed alkali matter
The 30-50% of amount, preferably 36-44%.In the usage ratio scope, preferable reaction effect is obtained in that,
Iridium loss late is low, Product yields are high.
Preferably, in step i), the reaction is entered at a temperature of 500-720 DEG C, preferably 600-700 DEG C
Row reaction.
It is further preferred that step i) is reacted by temperature programming, and preferably through following heating schedule
Reacted：
A. it is heated to 160-240 DEG C, preferably 200 DEG C ± 10% from room temperature, keeping temperature 10-60min, preferably
20-40min；
B. it is continuously heating to 460-540 DEG C, preferably 500 DEG C ± 5%, keeping temperature 10-60min, preferably
20-40min；It is preferred that 100-150 DEG C/h of heating rate；
C. 610-720 DEG C, preferably 650-700 DEG C is continuously heating to, 2-3.5h, preferably 2.5-3h is kept.
Preferably, 50-100 DEG C/h of the heating rate of heating schedule a.
Preferably, 100-150 DEG C/h of the heating rate of heating schedule b.
Preferably, 50-100 DEG C/h of the heating rate of heating schedule c.
By using above-mentioned reaction heating schedule, reacting balance can be made rapidly to carry out, both save reaction
Time can obtain preferable reaction result again.
In step i), preferably the mixture of iridium powder and mixed alkali is placed on crucible, then by crucible as height
Heating response in warm stove, such as Muffle furnace.
In certain preferred embodiments of the invention, in step ii) in, it is described stirring 56-75 DEG C, preferably
Carried out at 60-70 DEG C, preferably stirred 2-3 hours；Preferably, the consumption of the water is the 20-30 of mixed alkali quality
Times.
In step ii) in, the separation of solid and liquid is preferably heat filtering.
In step ii) in, the solid for preferably being obtained with the water washing separation of solid and liquid of mix alkali quality 20-30 times.
Iridium in the filtrate that the liquid and washing solid of separation of solid and liquid are produced is a small amount of iridium of loss.Of the invention
In method, by determining the amount of the iridium in the liquid and filtrate, the partial loss amount of iridium can be known.
In a preferred embodiment of the invention, in step iii) in, the quality of the chloroazotic acid is iridium silty amount
10-20 times, preferably 13-18 times.
In a preferred embodiment of the invention, step iii) described in react at 86-100 DEG C, preferably 90-99
Carried out at DEG C, the time of preferably described reaction is 3-5 hours.
By using the chloroazotic acid and reaction condition of above-mentioned amount, step ii can be made) in separation of solid and liquid produce consolidate
Body fully reacts as far as possible with chloroazotic acid.
Step iii) reaction mass cooling and separation of solid and liquid after, solid is unreacted iridium powder.Can be with less
Amount deionized water washing solid, the iridium powder for obtaining can be recycled.
In step iv) in, can as needed, by step iii) the liquid distillation and concentration that obtains of separation of solid and liquid is to one
Determine concentration, for example, distill the iridium content into Chloroiridic Acid solution for 20-30wt%, obtain required intermediate chlorine iridium
Acid.
Therefore, in the preferred embodiment of the invention, methods described also includes：By step iv) in separation of solid and liquid
The solid for obtaining is washed with water, and is reclaimed.
Preferably, the water used in step v) is 10-20 times of the weight of chloro-iridic acid product.
Preferably, in the alkali hydroxide soln, the concentration of alkali metal hydroxide is 20-40wt%,
It is preferred that 20-30wt%.The alkali metal hydroxide is preferably in potassium hydroxide, NaOH and lithium hydroxide
At least one.
Preferably, the liquid in step v) is titrated to pH value 8.6-10.3, preferably 9-10.Now produce big
The blue precipitate of amount, preferably heat filtering, i.e. step vi) in separation be preferably heat filtering mode.Obtain
Solid is preferably washed with deionized, filtering；The quality of the deionized water is preferably the 15-25 of mixed alkali quality
Times, preferably wash 3 times.The filtrate that heat filtering and washing are produced is merged, the iridium content in mixing filtrate is determined,
The a small amount of iridium for as losing, with reference to above-mentioned in step ii) after determine iridium loss amount, the present invention can be calculated
Prepare the total loss rate of the iridium in the method for acetic acid iridium.
In a preferred embodiment of the invention, in step vi) in, the aqueous 5-20wt% of aqueous acetic acid,
It is preferred that 8-14wt%.Preferably, the quality of the aqueous acetic acid is added the 20-40 of iridium silty amount by step i)
Times, preferably 26-34 times.It is further preferred that step vi) described in react time be 15-36 hours, preferably
20-28 hours.In this step, after after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium passes through
After vacuum distillation is concentrated to finite concentration, that is, acetic acid iridium product is obtained, acetic acid iridium catalyst can be directly used as.
In step vii) in, can as needed, by step vi) reaction mass distillation and concentration to finite concentration,
The iridium content into acetic acid iridium solution is for example distilled for more than 50wt%, obtains required acetic acid iridium product.
In the present invention, " separation of solid and liquid " is preferably filtering, such as filtration under diminished pressure, vacuum filter.
According to the present invention, a kind of method in fact providing coproduction chloro-iridic acid and acetic acid iridium.It is of the invention such as
In upper methods described, chloro-iridic acid can prepare the method mistake of acetic acid iridium as needed as intermediate product
Take out a part of chloro-iridic acid in journey, remaining part is then as the raw material for continuing to prepare acetic acid iridium.So, at this
Invent in the above method for providing, can simultaneously obtain chloro-iridic acid and acetic acid iridium product.
The preparation method of the acetic acid iridium that the present invention is provided has significant advantage：Building-up process is simple, iridium powder one way
High conversion rate, target product yield is high, and the loss late of iridium is low, such as ＜ 0.5%.It is well known that iridium powder is very
Expensive noble metal, therefore the making full use of of iridium powder, reduces loss late there are very prominent economic interests.
Specific embodiment
Explanation is further explained to the present invention with reference to specific embodiment, it should be appreciated that the scope of the present invention
Not limited to this.
Embodiment 1
In adding crucible after 12 grams of 4.5 grams of iridium powder and mixed alkali are sufficiently mixed.Mixed alkali is that mass ratio is 1:3 hydrogen
The solid mixture of sodium oxide molybdena and sodium peroxide.Crucible is put into Muffle furnace, is carried out according to following heating schedule
Reaction：
200 DEG C, keeping temperature half an hour, then with 120 are warmed up to 80 DEG C/h of heating rate from normal temperature
DEG C/h heating rate be warmed up to 500 DEG C, keeping temperature half an hour, then with 80 DEG C/h of intensification speed
Rate is warmed up to 650 DEG C, is kept for 2.5 hours, then natural cooling cooling.
During product washed into 250 ml deionized waters, stirred 2.5 hours at 60~70 DEG C.Cross while hot
Filter, filter cake is washed 3 times with 200 milliliters of deionized water, is filtered.Filtrate is merged, with ICP (inductance couplings
Plasma mass is closed, Agilent 7500cx, similarly hereinafter) iridium content in analysis filtrate, as a result to contain in filtrate
0.0095 gram of iridium.
By in filter cake 60 milliliters of chloroazotic acid of addition, 90~100 DEG C are heated to, stirring reaction 4 hours is filled with chloroazotic acid
Divide reaction.Cooled and filtered, filter cake is washed and filtered with a small amount of deionized water, and filter cake is unreacted iridium powder,
0.39 gram is weighed as after drying, can be recycled.Filtrate is concentrated in together, vacuum distillation is concentrated into chlorine iridium
Iridium content in acid solution is 25wt%, that is, obtain intermediate product chloro-iridic acid product.
Chloro-iridic acid product is dissolved in 150 ml deionized waters, under 75 DEG C of stirring states, with 25% hydrogen-oxygen
Change potassium solution titration, solution ph is titrated to 9.5, now produce a large amount of blue precipitates.Filter while hot, filter
Cake is washed 3 times with 150 ml deionized waters, filtering.The filtrate of the heat filtering and washing filtrate are merged, is used
Icp analysis iridium content, contains 0.0094 gram of iridium in filtrate.
During filter cake washed into aqueous 15% glacial acetic acid, the amount of glacial acetic acid is 160 milliliters, at reflux plus
Thermal response 24 hours, after after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium.By vacuum distillation
The iridium content in acetic acid iridium solution is concentrated to for more than 50wt%, that is, acetic acid iridium product is obtained.
It is computed, the conversion ratio of iridium is 91.3%, the loss late of iridium is 0.42%, wherein chloro-iridic acid preparatory phase
Iridium loss late be 0.21%.
Embodiment 2
In adding crucible after 12 grams of 5.0 grams of iridium powder and mixed alkali are sufficiently mixed.Mixed alkali is that mass ratio is 1:4 hydrogen
The solid mixture of sodium oxide molybdena and sodium peroxide.Crucible is put into Muffle furnace, is carried out according to following heating schedule
Reaction：
200 DEG C, keeping temperature half an hour, then with 120 are warmed up to 80 DEG C/h of heating rate from normal temperature
DEG C/h heating rate be warmed up to 500 DEG C, keeping temperature half an hour, then with 80 DEG C/h of intensification speed
Rate is warmed up to 680 DEG C, is kept for 2.5 hours, then natural cooling cooling.
During product washed into 250 ml deionized waters, stirred 2.5 hours at 60~70 DEG C.Cross while hot
Filter, filter cake is washed 3 times with 200 milliliters of deionized water, is filtered.Filtrate is merged, icp analysis filtrate is used
In iridium content, as a result in filtrate contain 0.0098 gram of iridium.
By in filter cake 60 milliliters of chloroazotic acid of addition, 90~100 DEG C are heated to, stirring reaction 4 hours is filled with chloroazotic acid
Divide reaction.Cooled and filtered, filter cake is washed and filtered with a small amount of deionized water, and filter cake is unreacted iridium powder,
0.45 gram is weighed as after drying, can be recycled.Filtrate is concentrated in together, vacuum distillation is concentrated into chlorine iridium
Iridium content in acid solution is 25wt% or so, that is, obtain intermediate product chloro-iridic acid product.
Chloro-iridic acid product is dissolved in 100 ml deionized waters, under 70~80 DEG C of stirring states, with 30%
Potassium hydroxide solution is titrated, and solution pH value is titrated into 9~10, now produces a large amount of blue precipitates.Cross while hot
Filter, filter cake is washed 3 times with 150 ml deionized waters, is filtered.The filtrate of the heat filtering and washing filtrate are closed
And, with icp analysis iridium content, 0.0096 gram of iridium is contained in filtrate.
During filter cake washed into aqueous 20% glacial acetic acid, the amount of glacial acetic acid is 120 milliliters, at reflux plus
Thermal response 24 hours, after after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium, by vacuum distillation
The iridium content in acetic acid iridium solution is concentrated to for more than 50wt%, that is, acetic acid iridium product is obtained.
It is computed, the conversion ratio of iridium is 91.0%, the loss amount of iridium is 0.39%, wherein chloro-iridic acid preparatory phase
Iridium loss late be 0.20%.
Embodiment 3
In adding crucible after 12 grams of 4.0 grams of iridium powder and mixed alkali are sufficiently mixed.Mixed alkali is that mass ratio is 1:2.5
The solid mixture of potassium hydroxide and potassium peroxide.Crucible is put into Muffle furnace, is entered according to following heating schedule
Row reaction：
200 DEG C, keeping temperature 20min, then with 120 are warmed up to 60 DEG C/h of heating rate from normal temperature
DEG C/h heating rate be warmed up to 500 DEG C, keeping temperature 40min, then with 90 DEG C/h of heating rate
700 DEG C are warmed up to, are kept for 3 hours, then natural cooling cooling.
During product washed into 300 ml deionized waters, stirred 2.5 hours at 60~70 DEG C.Cross while hot
Filter, filter cake is washed 3 times with 200 milliliters of deionized water, is filtered.Filtrate is merged, icp analysis filtrate is used
In iridium content, as a result in filtrate contain 0.0092 gram of iridium.
By in filter cake 45 milliliters of chloroazotic acid of addition, 96 DEG C are heated to, stirring reaction 3 hours is fully anti-with chloroazotic acid
Should.Cooled and filtered, filter cake is washed and filtered with a small amount of deionized water, and filter cake is unreacted iridium powder, is done
0.37 gram is weighed as after dry, can be recycled.Filtrate is concentrated in together, vacuum distillation is concentrated into chlorine iridium
Iridium content in acid solution is 25wt%, that is, obtain intermediate product chloro-iridic acid product.
Chloro-iridic acid product is dissolved in 100 ml deionized waters, under 70 DEG C of stirring states, with 30% hydrogen-oxygen
Change potassium solution titration, solution pH value is titrated to 10, now produce a large amount of blue precipitates.Filter while hot, filter
Cake is washed 3 times with 150 ml deionized waters, filtering.The filtrate of the heat filtering and washing filtrate are merged, is used
Icp analysis iridium content, contains 0.0091 gram of iridium in filtrate.
During filter cake washed into aqueous 20% glacial acetic acid, the amount of glacial acetic acid is 120 milliliters, at reflux plus
Thermal response 20 hours, after after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium, by vacuum distillation
The iridium content in acetic acid iridium solution is concentrated to for more than 50wt%, that is, acetic acid iridium product is obtained.
It is computed, the conversion ratio of iridium is 90.5%, the loss late of iridium is 0.46%, wherein chloro-iridic acid preparatory phase
Iridium loss late be 0.23%.
It can be seen that, chloro-iridic acid and/or the preparation method of acetic acid iridium that the present invention is provided, step is simple, iridium high conversion rate
And loss late is few, with considerable prospects for commercial application.
Although the present invention has been described in detail, it will be understood by those skilled in the art that in spirit of the invention and model
Modification in enclosing will be apparent.However, it should be understood that each side, difference that the present invention is recorded
The each several part of specific embodiment and the various features enumerated can be combined or all or part of exchange.Above-mentioned
Each specific embodiment in, those with reference to another embodiment implementation method can suitably with its
Its implementation method is combined, and this is will be to understand by those skilled in the art.Additionally, those skilled in the art
It will be understood that, description above is only the mode of example, it is no intended to the limitation present invention.
Claims (12)
1. a kind of preparation method of acetic acid iridium, the described method comprises the following steps：
I) iridium powder and mixed alkali are mixed and heated and are reacted；
Ii washed after the product cooling for) obtaining step i) in water, stirred, separation of solid and liquid；
Iii) by step ii) in separation of solid and liquid produce solid add chloroazotic acid in, heat and stir and reacted；
Iv) by step iii) reaction mass cool down and carry out separation of solid and liquid, then liquid distillation and concentration is obtained
Chloro-iridic acid product；
V) by step iv) obtain chloro-iridic acid product be added to the water, be titrated to alkali hydroxide soln
Alkalescence, produces precipitation；
Vi) the precipitate and separate for producing step v), and add aqueous acetic acid, heating reflux reaction；With
And
Vii) by step vi) reaction mass distillation and concentration, obtain acetic acid iridium.
2. preparation method according to claim 1, it is characterised in that the mixed alkali is alkali metal hydroxide
The solid mixture of thing and alkali-metal peroxide, preferably described alkali metal hydroxide and the alkali metal peroxide
The mass ratio of compound is 1:(1-5), preferably 1:(2-4), further preferably 1:(2.5-3.5).
3. preparation method according to claim 2, it is characterised in that the alkali metal hydroxide includes
At least one in NaOH, potassium hydroxide and lithium hydroxide, the alkali-metal peroxide includes peroxidating
At least one in sodium, potassium peroxide and lithium peroxide.
4. the preparation method according to any one of claim 1-3, it is characterised in that in step i),
The quality of the iridium powder is the 30-50%, preferably 36-44% of mixed alkali quality.
5. the preparation method according to any one of claim 1-4, it is characterised in that in step i),
The reaction is carried out at a temperature of 500-720 DEG C.
6. the preparation method according to any one of claim 1-5, it is characterised in that step i) passes through
Following heating schedule is reacted：
A. it is heated to 160-240 DEG C from room temperature, keeping temperature 10-60min, preferably 50-100 DEG C of heating rate/
Hour；
B. it is continuously heating to 460-540 DEG C, keeping temperature 10-60min, preferably 100-150 DEG C of heating rate/small
When；
C. 610-720 DEG C is continuously heating to, 2-3.5h, preferably 50-100 DEG C/h of heating rate is kept.
7. the preparation method according to any one of claim 1-6, it is characterised in that in step ii) in,
The stirring is carried out at 56-75 DEG C；And/or, the quality of the water is 20-30 times of mixed alkali quality；It is preferred that
The solid obtained with 20-30 times of mixed alkali quality of water washing separation of solid and liquid.
8. the preparation method according to any one of claim 1-7, it is characterised in that in step iii) in,
The quality of the chloroazotic acid is 10-20 times, preferably 13-18 times of iridium silty amount.
9. the preparation method according to any one of claim 1-8, it is characterised in that step iii) in institute
State reaction is carried out at 86-100 DEG C, and the time of preferably described reaction is 3-5 hours.
10. the preparation method according to any one of claim 1-9, it is characterised in that in step v),
In the alkali hydroxide soln, the concentration of alkali metal hydroxide is 10-40wt%, preferably 20-30
Wt%；The alkali metal hydroxide is preferably at least one in potassium hydroxide, NaOH and lithium hydroxide；
And/or
It is 8.6-10.3, preferably 9-10 that liquid in step v) is titrated to pH value.
11. preparation method according to any one of claim 1-10, it is characterised in that in step vi)
In, the aqueous 5-20wt% of aqueous acetic acid；And/or, the quality of the aqueous acetic acid is step i) institutes
Add 20-40 times, preferably 26-34 times of iridium silty amount；And/or, step vi) described in react time be
15-36 hours, preferably 20-28 hours.
12. preparation method according to any one of claim 1-11, it is characterised in that methods described is also
Including：By step iv) in the solid that obtains of separation of solid and liquid wash with water, and reclaim.
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| 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 |
| 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 |
| CN109293500A (en) * | 2018-10-19 | 2019-02-01 | 郴州高鑫铂业有限公司 | A kind of method of Microwave-assisted synthesis acetic acid iridium |
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