CN106335932A - Production process of ruthenium trichloride - Google Patents
Production process of ruthenium trichloride Download PDFInfo
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- CN106335932A CN106335932A CN201610759891.8A CN201610759891A CN106335932A CN 106335932 A CN106335932 A CN 106335932A CN 201610759891 A CN201610759891 A CN 201610759891A CN 106335932 A CN106335932 A CN 106335932A
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- ruthenium
- solution
- hydrochloric acid
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- ruthenium trichloride
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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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Abstract
The invention relates to a production process of ruthenium trichloride. According to the process, RuO4 gas is produced according to a traditional method; diluted hydrochloric acid is adopted for absorbing the RuO4 gas till the concentration of Ru in the solution ranges from 59 g/L to 61 g/L, meanwhile, the pH value is adjusted to range from 1.9 to 2.1, and a ruthenium-containing solution is obtained; a dispersing solvent is added into the ruthenium-containing solution, the adding volume of the dispersing solution is 9.8-10.2% of the volume of the ruthenium-containing solution, and the dispersed ruthenium-containing solution is obtained; the dispersing solvent is a mixture of hydrogen peroxide, ethyl alcohol and acetone according to the volume ratio of 1:(7.9-8.1):(0.95-1.05), the obtained dispersed ruthenium-containing solution is spray-dried through a spray dryer, and ruthenium trichloride powder is obtained. A traditional production process of ruthenium trichloride is improved, continuous, large-scale and equipment production is achieved, and the purposes of being short in production period, low in cost and free of polluting the environment are achieved.
Description
Technical field
The invention belongs to metal sorts technical field and in particular to a kind of production technology of ruthenium trichloride in Chemical Manufacture.
Background technology
With the continuous development of China's manufacture level, the selectivity that ruthenium catalyst is had, stability, catalysis activity
Require also to improve constantly.Be commonly used as at present presoma ruthenium compound product be mainly ruthenium trichloride, acetic acid ruthenium, ruthenium-oxide,
Nitric acid ruthenium.This product be widely used in petrochemical industry, chlorine industry, medical industry, perfume industry, environment-protection wastewater, waste gas and its
His precise electronic field, at present the consumption of domestic ruthenium catalyst convert into ruthenium meter and reached 50 tons/year.Industrial ruthenium catalyst can divide
For two classes, one be homogeneous catalyst be types of functionality type ruthenium compound, Typical Representative such as acetic acid ruthenium, ruthenium-oxide etc.;Two is carrier
Type catalyst, such as ruthenium carbon, ruthenium-iridium-tantalum net etc..Other also have ultra-fine ruthenium-oxide of used in electronic industry etc..Domestic ruthenium trichloride at present
Traditional processing technology is:
.
In traditional processing technology, because the concentration typically ratio of solution in concentration crystallization step is relatively low, need to be grown
The heating of time concentrates, so high energy consumption.Use in final crystallization simultaneously and toasted with glass container, will result in
Often a batch of homogeneity of product is poor.The tenor of product can only lean on the experience of workman to be controlled.Product crystallization
Grain is uneven, and in the industrial production, the product after drying is substantially bulk, and because production stage is more and energy consumption is higher,
So it is relatively costly.
Present patent application is directed to above-mentioned condition, has carried out the production Technology research and development of ruthenium trichloride, has been enabled with obtaining
Continuous prodution, good product consistency, low cost, reduces the production and processing technology of metal loss, provides for ruthenium catalyst industry
More reliable, using more convenient persursor material, extend rare precious metal industry industrial chain, fill a hole in the market, promote and produce
Industry develops.
Content of the invention
The problems referred to above existing aborning for current ruthenium trichloride, the present invention provides a kind of process is simple, produces week
Phase is short, low cost, free from environmental pollution, and water soluble acid dissolubility is good, the production technology of the stable ruthenium trichloride of ruthenium content.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of production technology of ruthenium trichloride, comprises the steps:
Step (1), conventionally produces ruo4Gas;Then dilute hydrochloric acid is adopted to absorb ruo4Gas, the ru to solution
Concentration is 59-61g/l, meanwhile, adjusts ph to 1.9-2.1, obtains containing ruthenium solution;
Described dilute hydrochloric acid be hydrochloric acid that mass fraction is 37% with water according to volume ratio (1.9-2.1): 1 mixes;
Step (2), to step (1) obtain containing in ruthenium solution add dispersion solvent, dispersion solvent add volume be molten containing ruthenium
Liquid amass 9.8-10.2%, after being disperseed containing ruthenium solution;
Described dispersion solvent is the mixture of hydrogen peroxide, ethanol and acetone, the body of hydrogen peroxide, ethanol and acetone in dispersion solvent
Long-pending ratio is 1:(7.9-8.1): (0.95-1.05);
Step (3), is spray-dried:
Being spray-dried using spray dryer containing ruthenium solution after the dispersion that step (2) is obtained, obtains ruthenium trichloride powder
End;
The temperature being spray-dried is 180-200 DEG C, and inlet amount is 800-1000ml/h;
The material of the nozzle of described spray dryer is politef.
It is further preferred that the regulation ph described in step (1) adopts aqueous hydrochloric acid solution.
It is further preferred that described aqueous hydrochloric acid solution be by mass fraction be 37% hydrochloric acid and water according to volume ratio
For 1:(3-4) mix.
It is further preferred that the nozzle diameter of described spray dryer is 0.5-2mm.
It is further preferred that in step (1), ruo is absorbed using dilute hydrochloric acid4Gas, to solution, the concentration of ru is
60g/l, meanwhile, adjusts ph to 2, obtains containing ruthenium solution;
Described dilute hydrochloric acid is that the hydrochloric acid that mass fraction is 37% is mixed according to volume ratio 2:1 with water.
It is further preferred that the volume that in step (2), dispersion solvent adds is 10% containing ruthenium solution volume.
It is further preferred that the volume ratio of hydrogen peroxide, ethanol and acetone is 1:8:1 in dispersion solvent.
It is further preferred that the described tail gas producing that is spray-dried adopts alkali liquor spray-absorption.Solution after absorption
The distilling apparatus that can directly return in traditional handicraft are circulated and distill.
It is further preferred that the mass concentration of described alkali liquor is 40%, that is, the mass concentration of sodium hydroxide is 40%.
The present invention carries out rapid draing crystallization to high concentration containing ruthenium solution using spray dryer.Can in crystallization process
To control the accuracy of temperature, obtain the stable product of stable ruthenium content it is achieved that the production of serialization mass.
Present invention spray dryer to be selected is preferably Automatic Control and Non-follow control two ore control pattern, and has
There is time set-up function, user need not manually can be guarded with the working time of sets itself machine, and the working time terminates machine and stops
Only work, need not manually guard, be greatly saved labour cost.
This spray dryer inlet temperature span of control is not less than 30 DEG C~300 DEG C this scopes.Preferably employ intelligent
Control system is higher to replace the control of the plc on market, stability;Intelligent control system best chromatic colour lcd touch screen is joined
Digital display shows, to show the parameters such as intake air temperature, air outlet temperature, wriggling revolution speed, air quantity;Using regulation and control pid thermostatic control
Technology, heated for controlling temperature precision: ± 1 DEG C, the product stability so produced is higher;The evaporated water scope of this spray dryer
Not less than this scope of 1500ml/h~2000ml/h;The inlet amount of this spray dryer is adjustable, and peristaltic pump adjustable extent is not little
In this scope of 50-2000ml/h.
Because spray drying device is universal standard equipment.The nozzle of equipment cannot bear the corruption of hydrochloric acid for common metal
Erosion.The present invention is improved to the nozzle material of equipment, thoroughly solves what nozzle was corroded using polytetrafluoroethylmaterial material
Situation occurs it is ensured that the quality of product.
In terms of tail gas recycle, applicant is solved using spray-absorption method by the final determination of substantial amounts of experiment work
Acid mist in tail gas is processed and micro ruthenium trichloride crystal reclaims problem, realizes the life of environmental protection, energy-conservation, serialization and mass
Produce.
The production technology of traditional ruthenium trichloride is by ruthenium powder and sodium hypochlorite reaction, and solution is in brownish black;B is to step a
Sulphuric acid is added, reaction generates golden yellow ruo4 gas in the solution generating;It is molten that the ruo4 gas that step b generates is passed through hydrochloric acid by c
In liquid, reaction generates ruthenium trichloride;Repeat step a and b, until solution is in water white transparency, finally by the ruthenium trichloride obtaining salt
Acid solution evaporative crystallization, obtains final product ruthenium trichloride.
The present invention in process of production, can realize the control of ruthenium content by changing baking temperature and inlet amount, this
Sample just can be controlled to the ruthenium content in product according to the special requirement of client, gives the special requirement meeting client.
Compared with prior art, its advantage is the present invention:
The production technology of traditional ruthenium trichloride is improved the present invention it is achieved that serialization, scale, equipment metaplasia product, reaches
Arrive with short production cycle, low cost, purpose free from environmental pollution, reduce the production loss causing because of production technology length.
The present invention passes through the adjustment of solution concentration and acidity and uses dispersion solvent, is carried out using spray drying device simultaneously
It is spray-dried, solve the problems, such as due to will result in metal loss technics comparing long production step in current traditional handicraft more,
Solve interpolation dispersant residue problem in the product simultaneously.
Dispersion solvent of the present invention can be quick and complete when 100 DEG C vaporization, and do not affect finally making of ruthenium trichloride product
With performance, the fast dewatering when being spray-dried crystallization can be made, thus the concordance realizing product is good.The crystal of product is uniform
The good purpose of property.
Compared with traditional handicraft, without condensing crystallizing, can get the stable powdery product of batch.Compare traditional handicraft,
Loss can reduce at least 60%.
Present invention determine that ruthenium trichloride batch crystallisation technological parameter, product, product ruthenium content >=37%, water can be prepared in batches
Dissolubility and acid-soluble all preferable, product granularity is -60 mesh, and properties of product are stable, and concordance is good, reaches making of catalyst precursor
With requiring.
The present invention has carried out technological improvement to traditional spray drying device, to meet the need that ruthenium trichloride of the present invention produces
Ask.
It is directly powder that the present invention obtains ruthenium trichloride product, and this largely avoided block ruthenium trichloride and carries when using
The inconvenience coming, and when using, the deliquescence problem that long subpackage, weighing bring, this is for the using effect of subsequent clients
Give very big lifting.Because many experiments preferably must be held in anhydrous under the conditions of carry out, if the trichlorine as catalyst
Change ruthenium by deliquescence, then can affect experiment effect.
In terms of tail gas recycle, applicant is solved using spray-absorption method by the final determination of substantial amounts of experiment work
Acid mist in tail gas is processed and micro ruthenium trichloride Product recycling problem, realizes the life of environmental protection, energy-conservation, serialization and mass
Produce.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and should not be regarded as limiting this
Bright scope.Unreceipted particular technique or condition person in embodiment, according to the technology described by document in the art or condition
Or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, are and can pass through what purchase obtain
Conventional products.
Embodiment 1
A kind of production technology of ruthenium trichloride, comprises the steps:
Step (1), conventionally produces ruo4Gas;Then dilute hydrochloric acid is adopted to absorb ruo4Gas, the ru to solution
Concentration is 59g/l, meanwhile, adjusts ph to 1.9, obtains containing ruthenium solution;
Described dilute hydrochloric acid is that the hydrochloric acid that mass fraction is 37% is mixed according to volume ratio 1.9:1 with water;
Step (2), to step (1) obtain containing in ruthenium solution add dispersion solvent, dispersion solvent add volume be molten containing ruthenium
Liquid amass 9.8%, after being disperseed containing ruthenium solution;
Described dispersion solvent is the mixture of hydrogen peroxide, ethanol and acetone, the body of hydrogen peroxide, ethanol and acetone in dispersion solvent
Long-pending ratio is 1:7.9:0.95;
Step (3), is spray-dried:
Being spray-dried using spray dryer containing ruthenium solution after the dispersion that step (2) is obtained, obtains ruthenium trichloride powder
End;
The temperature being spray-dried is 180-200 DEG C, and inlet amount is 800-1000ml/h;
The material of the nozzle of described spray dryer is politef.The nozzle diameter of described spray dryer is
0.5mm.
Embodiment 2
A kind of production technology of ruthenium trichloride, comprises the steps:
Step (1), conventionally produces ruo4Gas;Then dilute hydrochloric acid is adopted to absorb ruo4Gas, the ru to solution
Concentration is 61g/l, meanwhile, adjusts ph to 1.9-2.1, obtains containing ruthenium solution;
Described dilute hydrochloric acid is that the hydrochloric acid that mass fraction is 37% is mixed according to volume ratio 2.1:1 with water;
Step (2), to step (1) obtain containing in ruthenium solution add dispersion solvent, dispersion solvent add volume be molten containing ruthenium
Liquid amass 10.2%, after being disperseed containing ruthenium solution;
Described dispersion solvent is the mixture of hydrogen peroxide, ethanol and acetone, the body of hydrogen peroxide, ethanol and acetone in dispersion solvent
Long-pending ratio is 1:8.1:1.05;
Step (3), is spray-dried:
Being spray-dried using spray dryer containing ruthenium solution after the dispersion that step (2) is obtained, obtains ruthenium trichloride powder
End;
The temperature being spray-dried is 180-200 DEG C, and inlet amount is 800-1000ml/h;
The material of the nozzle of described spray dryer is politef.The nozzle diameter of described spray dryer is 2mm.
Regulation ph described in step (1) adopts aqueous hydrochloric acid solution.Described aqueous hydrochloric acid solution be by mass fraction be 37%
Hydrochloric acid mix for 1:3 according to volume ratio with water.
Embodiment 3
A kind of production technology of ruthenium trichloride, comprises the steps:
Step (1), conventionally produces ruo4Gas;Then dilute hydrochloric acid is adopted to absorb ruo4Gas, the ru to solution
Concentration is 60g/l, meanwhile, adjusts ph to 2, obtains containing ruthenium solution;
Described dilute hydrochloric acid is that the hydrochloric acid that mass fraction is 37% is mixed according to volume ratio 2:1 with water;
Step (2), to step (1) obtain containing in ruthenium solution add dispersion solvent, dispersion solvent add volume be molten containing ruthenium
Liquid amass 10%, after being disperseed containing ruthenium solution;
Described dispersion solvent is the mixture of hydrogen peroxide, ethanol and acetone, the body of hydrogen peroxide, ethanol and acetone in dispersion solvent
Long-pending ratio is 1:8:1;
Step (3), is spray-dried:
Being spray-dried using spray dryer containing ruthenium solution after the dispersion that step (2) is obtained, obtains ruthenium trichloride powder
End;
The temperature being spray-dried is 180-200 DEG C, and inlet amount is 800-1000ml/h;
The material of the nozzle of described spray dryer is politef.The nozzle diameter of described spray dryer is 1mm.
Regulation ph described in step (1) adopts aqueous hydrochloric acid solution.Described aqueous hydrochloric acid solution be by mass fraction be 37%
Hydrochloric acid mix for 1:4 according to volume ratio with water.
It is spray-dried the tail gas producing and adopt alkali liquor spray-absorption.
Embodiment 4
Embodiment 4 is with the difference of embodiment 3:
Regulation ph described in step (1) adopts aqueous hydrochloric acid solution.The salt that described aqueous hydrochloric acid solution is is 37% by mass fraction
Acid is mixed for 1:3.5 according to volume ratio with water.It is spray-dried the alkali liquor spray that the tail gas producing is 40% using mass concentration
Absorb.
Remaining is all identical.
Comparative example 1
Comparative example 1 is with the difference of embodiment 3: the concentration containing ruthenium solution ru in step (1) is 100g/l, and remaining is all identical.
Prepared product ruthenium content is low, and is dried not exclusively.
Comparative example 2
Comparative example 2 is with the difference of embodiment 3: the concentration containing ruthenium solution ru in step (1) is 30g/l, and remaining is all identical.
Prepared product ruthenium content is too high, and yield is relatively low, deficiency in economic performance.
Comparative example 3
Comparative example 3 is with the difference of embodiment 3: no step (2) adds dispersion solvent step, and remaining is all identical.
Substantial amounts of caking in prepared product, and economic benefit is decreased obviously.
Comparative example 4
Comparative example 4 is with the difference of embodiment 3: the temperature of spray drying is 110 DEG C.
Prepared product drying is incomplete, and yield declines to a great extent, and at least declines 10%.
Ultimate principle, principal character and the advantages of the present invention of the present invention have been shown and described above.The technology of the industry
, it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description is originally for personnel
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and its
Equivalent thereof.
Claims (9)
1. a kind of production technology of ruthenium trichloride is it is characterised in that comprise the steps:
Step (1), conventionally produces ruo4Gas;Then dilute hydrochloric acid is adopted to absorb ruo4Gas, to solution, ru's is dense
Spend for 59-61g/l, meanwhile, adjust ph to 1.9-2.1, obtain containing ruthenium solution;
Described dilute hydrochloric acid be hydrochloric acid that mass fraction is 37% with water according to volume ratio (1.9-2.1): 1 mixes;
Step (2), to step (1) obtain containing in ruthenium solution add dispersion solvent, dispersion solvent add volume be molten containing ruthenium
Liquid amass 9.8-10.2%, after being disperseed containing ruthenium solution;
Described dispersion solvent is the mixture of hydrogen peroxide, ethanol and acetone, the body of hydrogen peroxide, ethanol and acetone in dispersion solvent
Long-pending ratio is 1:(7.9-8.1): (0.95-1.05);
Step (3), is spray-dried:
Being spray-dried using spray dryer containing ruthenium solution after the dispersion that step (2) is obtained, obtains ruthenium trichloride powder
End;
The temperature being spray-dried is 180-200 DEG C, and inlet amount is 800-1000ml/h;
The material of the nozzle of described spray dryer is politef.
2. the production technology of ruthenium trichloride according to claim 1 is it is characterised in that the regulation ph described in step (1)
Using aqueous hydrochloric acid solution.
3. the production technology of ruthenium trichloride according to claim 2 is it is characterised in that described aqueous hydrochloric acid solution is by matter
Amount fraction is 37% hydrochloric acid is 1:(3-4 with water according to volume ratio) mix.
4. the production technology of ruthenium trichloride according to claim 1 is it is characterised in that the nozzle of described spray dryer
Bore is 0.5-2mm.
5. the production technology of ruthenium trichloride according to claim 1 is it is characterised in that in step (1), inhaled using dilute hydrochloric acid
Receive ruo4Gas, to solution, the concentration of ru is 60g/l, meanwhile, adjusts ph to 2, obtains containing ruthenium solution;
Described dilute hydrochloric acid is that the hydrochloric acid that mass fraction is 37% is mixed according to volume ratio 2:1 with water.
6. ruthenium trichloride according to claim 1 production technology it is characterised in that in step (2) dispersion solvent add
Volume be containing ruthenium solution volume 10%.
7. the production technology of ruthenium trichloride according to claim 1 is it is characterised in that hydrogen peroxide, ethanol in dispersion solvent
Volume ratio with acetone is 1:8:1.
8. the production technology of ruthenium trichloride according to claim 1 is it is characterised in that described is spray-dried the tail producing
Gas adopts alkali liquor spray-absorption.
9. the production technology of ruthenium trichloride according to claim 8 is it is characterised in that the mass concentration of described alkali liquor is
40%.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107162069A (en) * | 2017-05-12 | 2017-09-15 | 常州大学 | The recovery process of ruthenium trichloride catalyst in a kind of trimethyl pyruvic acid synthesis procedure |
CN110255632A (en) * | 2019-07-17 | 2019-09-20 | 江西省汉高新材料有限公司 | The method for preparing ruthenium trichloride with waste material containing ruthenium |
CN114717642A (en) * | 2022-04-13 | 2022-07-08 | 徐州浩通新材料科技股份有限公司 | Method for preparing high-purity ruthenium trichloride crystal from crude ruthenium solution |
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CN101891261A (en) * | 2010-08-31 | 2010-11-24 | 郴州高鑫铂业有限公司 | Method for preparing ruthenium trichloride from coarse ruthenium powder |
CN103626240A (en) * | 2013-12-15 | 2014-03-12 | 郴州高鑫铂业有限公司 | Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid |
WO2014091456A1 (en) * | 2012-12-14 | 2014-06-19 | Fer-Min-Ore (Proprietary) Limited | Process for recovering platinum group metals |
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CN101462778A (en) * | 2007-12-20 | 2009-06-24 | 中国蓝星(集团)股份有限公司 | Preparation of ruthenium trichloride |
CN101891261A (en) * | 2010-08-31 | 2010-11-24 | 郴州高鑫铂业有限公司 | Method for preparing ruthenium trichloride from coarse ruthenium powder |
WO2014091456A1 (en) * | 2012-12-14 | 2014-06-19 | Fer-Min-Ore (Proprietary) Limited | Process for recovering platinum group metals |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107162069A (en) * | 2017-05-12 | 2017-09-15 | 常州大学 | The recovery process of ruthenium trichloride catalyst in a kind of trimethyl pyruvic acid synthesis procedure |
CN110255632A (en) * | 2019-07-17 | 2019-09-20 | 江西省汉高新材料有限公司 | The method for preparing ruthenium trichloride with waste material containing ruthenium |
CN110255632B (en) * | 2019-07-17 | 2021-05-25 | 江西省汉氏贵金属有限公司 | Method for preparing ruthenium trichloride from ruthenium-containing waste |
CN114717642A (en) * | 2022-04-13 | 2022-07-08 | 徐州浩通新材料科技股份有限公司 | Method for preparing high-purity ruthenium trichloride crystal from crude ruthenium solution |
CN114717642B (en) * | 2022-04-13 | 2023-11-10 | 徐州浩通新材料科技股份有限公司 | Method for preparing high-purity ruthenium trichloride crystals from crude ruthenium solution |
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