CN106807445A - A kind of preparation method of acetic acid iridium catalyst - Google Patents
A kind of preparation method of acetic acid iridium catalyst Download PDFInfo
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- CN106807445A CN106807445A CN201510847917.XA CN201510847917A CN106807445A CN 106807445 A CN106807445 A CN 106807445A CN 201510847917 A CN201510847917 A CN 201510847917A CN 106807445 A CN106807445 A CN 106807445A
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- iridium
- acetic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Abstract
The invention provides a kind of preparation method of acetic acid iridium catalyst, the described method comprises the following steps:A) iridium powder and mixed alkali are mixed and heated and are reacted;B) product for obtaining step a) is washed in hydrochloric acid after cooling down, stirring reaction;C) to chloroazotic acid is added in the reaction stream of step b), stirring reaction is continued, then separation of solid and liquid;D) liquid for being obtained with separation of solid and liquid in alkali hydroxide soln titration step c) produces precipitation to alkalescence;E) precipitate and separate for producing step d), and wash aqueous acetic acid, heating reflux reaction;And f) by the reaction mass distillation and concentration of step e), obtain acetic acid iridium catalyst.The preparation method of the acetic acid iridium catalyst that the present invention is provided, building-up process is simple, and iridium powder conversion per pass is high, and 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 catalyst, and in particular to a kind of preparation of acetic acid iridium catalyst
Method.
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 is prepared into chloro-iridic acid by series reaction,
Typically metal iridium powder and basic anhydride are reacted in high temperature furnace, product is dissolved in acid, through filtering
Unreacted iridium powder is isolated in washing, and ammonium chloroiridate is obtained with ammonium chloride reaction again after gained filtrate and chloroazotic acid reaction
Precipitation, the ammonium chloroiridate obtained after filtration washing is concentrated to give chloro-iridic acid with chloroazotic acid reaction again;Then again by chlorine
Iridium acid prepares acetic acid iridium catalyst by series reaction.This acetic acid iridium preparation process is complicated, and iridium damage
Lose 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 preparation method of acetic acid iridium catalyst, the described method comprises the following steps:
A) iridium powder and mixed alkali are mixed and heated and are reacted;
B) product for obtaining step a) is washed in hydrochloric acid after cooling down, stirring reaction;
C) to chloroazotic acid is added in the reaction stream of step b), stirring reaction is continued, then separation of solid and liquid;
D) liquid for being obtained with separation of solid and liquid in alkali hydroxide soln titration step c) is produced to alkalescence
Precipitation;
E) precipitate and separate for producing step d), and wash aqueous acetic acid, heating reflux reaction;And
F) by the reaction mass distillation and concentration of step e), acetic acid iridium catalyst is obtained.
According to the present invention, after iridium powder and mixed alkali are reacted, dissolving with hydrochloric acid product is first added, add chloroazotic acid
Reaction produces chloro-iridic acid, is then directly added into alkaline reaction, then is obtained with acetum reaction after solid is separated
Acetic acid iridium product.It can be seen that, the present invention by the middle chloro-iridic acid separating-purifying for producing, and need not directly be settled at one go
Generation acetic acid iridium.Compared with prior art, in the course of reaction of the inventive method, without utilizing ammonium chloride
Reaction is obtained after ammonium chloroiridate, just produces chloro-iridic acid with chloroazotic acid reaction again.It can be seen that, the side that the present invention is provided
Method is simpler than existing method, and saves reagent, reduces the generation of waste liquid.Additionally, the reduction of method and step for
Significant advantage can be brought for noble metal reaction, because the reduction of step can reduce the loss of noble metal
Amount, 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 a), 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 a), 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 a), the reaction is entered at a temperature of 500-720 DEG C, preferably 600-700 DEG C
OK.
It is further preferred that step a) is reacted by temperature programming, and preferably through following heating schedule
Reacted:
I. it is heated to 160-240 DEG C, preferably 200 DEG C ± 10% from room temperature, keeping temperature 10-60min, preferably
20-40min;
Ii. 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;
Iii. 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 i.
Preferably, 100-150 DEG C/h of the heating rate of heating schedule ii.
Preferably, 50-100 DEG C/h of the heating rate of heating schedule iii.
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 a), 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.
According to the present invention, in step step b), the concentration of the hydrochloric acid is 11.0-12.5mol/L, preferably institute
Hydrochloric acid is stated for concentrated hydrochloric acid.
Preferably, the consumption of hydrochloric acid is 5-15 times of the mixed alkali quality.
Preferably, the temperature reacted described in step b) is 66-84 DEG C, preferably 70-80 DEG C;It is preferred that when reacting
Between 1-3 hours.
By first adding appropriate concentrated hydrochloric acid, iridium powder can be made to be dissolved as much as possible with the product of mixed alkali,
Then adding chloroazotic acid makes the product further fully dissolve, and adds the chloroazotic acid can also to stablize iridium
Valence state, while the consumption of chloroazotic acid can also be reduced.Therefore, step b) and setting c) has for reaction result
It is significant.
In a preferred embodiment of the invention, in step c), the consumption of chloroazotic acid is the mixed alkali quality
2-5 times.Preferably, the temperature reacted described in step c) is 76-94 DEG C, preferably 80-90 DEG C;It is preferred that reacting
Time be 1-2 hours.
Preferably, in step c), after fully reaction, separation of solid and liquid is carried out again after appropriate cooling.It is preferred that
Solid is washed with a small amount of deionized water.The solid is unreacted iridium powder, can recycle.
Therefore, in a preferred embodiment of the invention, the method that the present invention is provided also includes:By step c)
The solid that middle separation of solid and liquid is obtained is washed with water, and is reclaimed.
In a preferred embodiment of the invention, also the liquid that separation of solid and liquid in step c) is obtained is distilled,
With recovery acid, concentrate alkali hydroxide soln is then titrated to alkalescence again, produces precipitation.
Preferably, in step d), the concentration of the alkali hydroxide soln is 20-40wt%, preferably
20-30wt%;The alkali metal hydroxide is preferably in potassium hydroxide, NaOH and lithium hydroxide at least
It is a kind of.
Preferably, the liquid in step d) is titrated to pH value 8.6-10.3, preferably 9-10.Now produce big
Separation in the blue precipitate of amount, preferably heat filtering, i.e. step e) is preferably the mode of heat filtering.Obtain
Solid is preferably washed with deionized, filtering;The consumption 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, can calculate the loss late of the iridium in the inventive method.
In a preferred embodiment of the invention, in step e), the aqueous 5-20wt% of aqueous acetic acid,
It is preferred that 8-14wt%.Preferably, the consumption of the aqueous acetic acid is added the 20-40 of iridium silty amount by step a)
Times, preferably 26-34 times.It is further preferred that the time reacted described in step e) is 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 catalyst is obtained.
In step f), can as needed, by the reaction mass distillation and concentration of step d) 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.
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 < 0.3%.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 100 milliliters of concentrated hydrochloric acids, stirred 2 hours at 70~80 DEG C.Add chloroazotic acid
30 milliliters, stirred 1.5 hours at 80~90 DEG C, product is fully dissolved.
The appropriate cooled and filtered of reaction mass, filter cake is washed with a small amount of deionized water, and filter cake is unreacted iridium
Powder, 0.39 gram is weighed as after drying, and can be recycled.All filtrates are concentrated in together, Distillation recovery acid.
Then, by concentrate under 70~80 DEG C of stirring states, pH value 9.3 is titrated to 30% potassium hydroxide solution,
Now produce a large amount of blue precipitates.Filter while hot, filter cake is washed 3 times with 200 milliliters of deionized water every time,
Filtering;The filtrate of the heat filtering and washing filtrate are merged, with ICP (inductivity coupled plasma mass spectrometry, peace
Prompt human relations 7500cx, similarly hereinafter) analysis iridium content, as a result to contain 0.0095 gram of iridium in filtrate.
During filter cake to wash aqueous 10% 150 milliliters of glacial acetic acid, heating response 24 hours at reflux,
After after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium is concentrated to acetic acid iridium solution by vacuum distillation
In iridium content be, for example, more than 50wt%, that is, acetic acid iridium catalyst is obtained.
It is computed, the conversion ratio of iridium is 91.3%, the loss late of iridium is 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:
Be warmed up to 200 DEG C with 80 DEG C/h of heating rate from normal temperature, keeping temperature half an hour, then with 120 DEG C/
The heating rate of hour is warmed up to 500 DEG C, keeping temperature half an hour, then with 80 DEG C/h of heating rate liter
Temperature is kept for 2.5 hours, then natural cooling cooling to 680 DEG C.
During product washed into 100 milliliters of concentrated hydrochloric acids, stirred 2 hours at 70~80 DEG C.Add chloroazotic acid
30 milliliters, stirred 1.5 hours at 80~90 DEG C, product is fully dissolved.
The appropriate cooled and filtered of reaction mass, filter cake is washed with a small amount of deionized water, and filter cake is unreacted iridium
Powder, 0.45 gram is weighed as after drying, and can be recycled.All filtrates are concentrated in together, Distillation recovery acid.
Then concentrate is titrated to pH value 9.6 under 70~80 DEG C of stirring states with 30% sodium hydroxide solution, this
When produce a large amount of blue precipitates.Filter while hot, filter cake washs 3 times, mistake with 200 milliliters of deionized water every time
Filter;The filtrate of the heat filtering and washing filtrate are merged, with icp analysis iridium content, as a result to contain iridium in filtrate
0.0098 gram.
During filter cake to wash aqueous 14% 150 milliliters of glacial acetic acid, heating response 20 hours at reflux,
After after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium is concentrated to acetic acid iridium solution by vacuum distillation
In iridium content be more than 50wt%, that is, acetic acid iridium catalyst is obtained.
It is computed, the conversion ratio of iridium is 91.0%, the loss late of iridium is 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 120 milliliters of concentrated hydrochloric acids, stirred 3 hours at 80 DEG C.Add chloroazotic acid 40
Milliliter, is stirred 1.5 hours at 80~90 DEG C, and product is fully dissolved.
The appropriate cooled and filtered of reaction mass, filter cake is washed with a small amount of deionized water, and filter cake is unreacted iridium
Powder, 0.37 gram is weighed as after drying, and can be recycled.All filtrates are concentrated in together, Distillation recovery acid.
Then concentrate is titrated to pH value 9~10 under 70~80 DEG C of stirring states with 25% sodium hydroxide solution,
Now produce a large amount of blue precipitates.Filter while hot, filter cake is washed 3 times with 200 milliliters of deionized water every time,
Filtering;The filtrate of the heat filtering and washing filtrate are merged, with icp analysis iridium content, as a result to contain in filtrate
0.0088 gram of iridium.
During filter cake to wash aqueous 14% 150 milliliters of glacial acetic acid, heating response 20 hours at reflux,
After after solid all dissolving, the as glacial acetic acid solution of acetic acid iridium is concentrated to acetic acid iridium solution by vacuum distillation
In iridium content be more than 50wt%, that is, acetic acid iridium catalyst is obtained.
It is computed, the conversion ratio of iridium is 90.7%, the loss late of iridium is 0.22%.
It can be seen that, the acetic acid iridium preparation method 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 (11)
1. a kind of preparation method of acetic acid iridium catalyst, the described method comprises the following steps:
A) iridium powder and mixed alkali are mixed and heated and are reacted;
B) product for obtaining step a) is washed in hydrochloric acid after cooling down, stirring reaction;
C) to chloroazotic acid is added in the reaction stream of step b), stirring reaction is continued, then separation of solid and liquid;
D) liquid for being obtained with separation of solid and liquid in alkali hydroxide soln titration step c) is produced to alkalescence
Precipitation;
E) precipitate and separate for producing step d), and wash aqueous acetic acid, heating reflux reaction;And
F) by the reaction mass distillation and concentration of step e), acetic acid iridium catalyst is obtained.
2. preparation method according to claim 1, it is characterised in that the mixed alkali is alkali metal hydroxide
With the solid mixture of alkali-metal peroxide, preferably described alkali metal hydroxide and the alkali-metal peroxide
The mass ratio of thing 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 a),
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 a),
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 a) passes through
Following heating schedule is reacted:
I. it is heated to 160-240 DEG C from room temperature, keeping temperature 10-60min, preferably 50-100 DEG C of heating rate/
Hour;
Ii. it is continuously heating to 460-540 DEG C, keeping temperature 10-60min, preferably 100-150 DEG C of heating rate/small
When;
Iii. 610-720 DEG C is continuously heating to, 2-3.5h, preferably 50-100 DEG C/h of heating rate is kept.
7. the method according to any one of claim 1-6, it is characterised in that in step b), institute
The concentration for stating hydrochloric acid is 11.0-12.5mol/L;And/or, the consumption of hydrochloric acid is 5-15 times of the mixed alkali quality;
And/or, the temperature reacted described in step b) is 66-84 DEG C, preferred reaction time 1-3 hours.
8. the method according to any one of claim 1-7, it is characterised in that in step c), king
The consumption of water is 2-5 times of the mixed alkali quality;And/or, the temperature reacted described in step c) is 76-94
DEG C, the time preferably reacted is 1-2 hours.
9. the method according to any one of claim 1-8, it is characterised in that in step d), institute
State in alkali hydroxide soln, the concentration of alkali metal hydroxide is 10-40wt%, preferably 20-30wt%;
The alkali metal hydroxide is preferably at least one in potassium hydroxide, NaOH and lithium hydroxide;With/
Or
It is 8.6-10.3, preferably 9-10 that liquid in step d) is titrated to pH value.
10. the method according to any one of claim 1-9, it is characterised in that in step e), institute
State the aqueous 5-20wt% of aqueous acetic acid;And/or, the consumption of the aqueous acetic acid adds iridium by step a)
20-40 times of silty amount, preferably 26-34 times;And/or, the time reacted described in step e) is 15-36
Hour, preferably 20-28 hours.
11. preparation method according to any one of claim 1-10, it is characterised in that methods described is also
Including:The solid that separation of solid and liquid in step c) is obtained is washed with water, and is reclaimed.
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Cited By (3)
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CN108409554A (en) * | 2018-03-28 | 2018-08-17 | 西安瑞鑫科金属材料有限责任公司 | A kind of synthetic method of acetic acid iridium |
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 |
CN112439437A (en) * | 2019-08-28 | 2021-03-05 | 中国石油化工股份有限公司 | Iridium-containing solution as catalyst for synthesizing acetic acid, and preparation method and application thereof |
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GB2413323A (en) * | 2004-04-22 | 2005-10-26 | Johnson Matthey Plc | Improvements to processes for the preparation of iridium acetate |
CN101213165A (en) * | 2005-05-25 | 2008-07-02 | 尤米科尔股份公司及两合公司 | Process for the preparation of iridium acetate |
CN101445872A (en) * | 2007-11-27 | 2009-06-03 | 中国蓝星(集团)股份有限公司 | Method for extracting noble metal iridium from mixed oxide containing ruthenium, iridium, titanium, tin, zirconium and palladium |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108409554A (en) * | 2018-03-28 | 2018-08-17 | 西安瑞鑫科金属材料有限责任公司 | A kind of synthetic method of acetic acid iridium |
CN108409554B (en) * | 2018-03-28 | 2021-04-20 | 西安瑞鑫科金属材料有限责任公司 | Synthetic method of iridium acetate |
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 |
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 |
CN112439437A (en) * | 2019-08-28 | 2021-03-05 | 中国石油化工股份有限公司 | Iridium-containing solution as catalyst for synthesizing acetic acid, and preparation method and application thereof |
CN112439437B (en) * | 2019-08-28 | 2023-08-15 | 中国石油化工股份有限公司 | Iridium-containing solution used as catalyst for synthesizing acetic acid, and preparation method and application thereof |
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