CN103626240A - Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid - Google Patents
Method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid Download PDFInfo
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Abstract
The invention provides a method for preparing ruthenium trichloride with low-concentration complicated ruthenium-containing waste liquid. The method comprises the steps that the low-concentration complicated ruthenium-containing waste liquid is subjected to acidification, selective ruthenium settlement and routine washing and drying; enriched ruthenium residues are obtained; the ruthenium residues are subjected to chlorine alkalization distillation, hydrochloric acid absorption, concentration and baking; and reagent-grade ruthenium trichloride is prepared. The method has the characteristics that a technology is simple; the energy consumption is low; a ruthenium enrichment rate is high; an impurity element reaches the standard; the distillation times are less; the reaction time is short; the product quality is easy to control; and a product yield is high.
Description
Technical field
The invention belongs to field of fine chemical, relate to a kind of complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration.
Background technology
Ruthenium trichloride is one of most important compound of ruthenium, is the important industrial chemicals in the fields such as heterogeneous catalyst, homogeneous catalysis, plating, coating.Ruthenium trichloride is the main raw material of electric tank metal anode coating, in China, produced more than 20 year, family more than 30 of the existing electrolyzer manufacturing enterprise of China, metal anode is in electrochemical field widespread uses such as chlorine industry, inorganic electrosynthesis, Organic Electricity are synthetic, metallurgical, and wherein 95% of chlorine industry septation method caustic soda is that applied metal anode electrolytic tank is produced.
China's ruthenium natural resources shortage, producing ruthenium amount per year only has tens kilograms, and less than 1% of demand, therefore, the regeneration of the secondary resource of ruthenium is recycled significant.How from secondary resource, to extract ruthenium and become the focus that China practitioner pays close attention to, from electrolyzer, reclaiming ruthenium, to prepare ruthenium trichloride be also one of emphasis, at present, lower concentration is complicated adopts the method for common neutralization--charcoal absorption-burning enrichment conventionally containing ruthenium waste liquid, or use strong reductant direct-reduction, these two kinds of methods all have complex process, energy consumption is high, ruthenium accumulation rate is low, the shortcomings such as the many and contaminate environment of impurity element, simultaneously conventionally adopt sodium chlorate to add sulfuric acid system preparing ruthenium trichloride, exist distillation often, long reaction time, the difficult control of quality product, the problems such as product yield is low.
Summary of the invention
The object of this invention is to provide a kind of complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration.Wherein the complicated process containing ruthenium waste liquid enrichment ruthenium of lower concentration has solved complex process, energy consumption is high, ruthenium accumulation rate is low, impurity element many and the shortcoming such as contaminate environment, the preparation of ruthenium trichloride adopts the production technique of chlorine hydro-oxidation sodium to improve quality product, has shortened the reaction times.
In order to achieve the above object, Technical Design of the present invention is as follows:
The complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration, is characterized in that: lower concentration complicated containing ruthenium waste liquid through acidifying, the heavy ruthenium of selectivity, through the dry ruthenium slag that obtains enrichment of routine washing; Ruthenium slag adds alkali distillation, absorption by Hydrochloric Acid, the concentrated ruthenium trichloride that is prepared into SILVER REAGENT that toasts through chlorine.
The complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration, it is characterized in that, lower concentration is complicated is containing in ruthenium waste liquid, to add one or both mixing acid in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, the 1-15% that concentration is waste liquid to lower concentration is complicated containing the acidifying of ruthenium waste liquid.
lower concentration is complicated prepares ruthenium trichloride containing ruthenium waste liquid, it is characterized in that, the heavy ruthenium of selectivity is a kind of precipitation agent adding in solution in ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, 1 times of thin up, the consumption of precipitation agent is 0.5-10 times of ruthenium quality.
The complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration, it is characterized in that, ruthenium slag adds through chlorine the ruthenium trichloride that alkali distillation, absorption by Hydrochloric Acid, concentrated baking be prepared into SILVER REAGENT and follows these steps to carry out: 1. under air-tight state negative pressure to add massfraction be the NaOH solution of 20-40%, the material proportion of thick ruthenium powder and sodium hydroxide solution is 1: 10 – 100; 2. be heated to 80 ℃, to step, pass into chlorine in 1., passing into chlorine flowrate is 50 – 120mL/min, controls temperature of reaction at 105 ℃, generates yellow RuO
4gas; 3. the RuO 2. step being generated
4gas is through deionized water purifying, passing into multistage absorption by Hydrochloric Acid liquid absorbs, concentration of hydrochloric acid is 2-10mol/L, temperature control is 25-40 ℃, in absorption by Hydrochloric Acid liquid, add reductive agent, reductive agent is a kind of or two kinds of mixtures of methyl alcohol, ethanol, n-propyl alcohol, Virahol, and the massfraction of reductive agent is 0.01 – 6%, and reaction generates red-brown H
2ruCl
5solution, tail gas passes into 15% NaOH solution absorption through negative pressure; 4. the H 3. step being generated
2ruCl
5, crystallization concentrated through conventional heating and infrared drying obtain the RuCl of chocolate
3crystal.
The inventive method, the lower concentration of take is complicated is raw material containing ruthenium waste liquid, acidifying, selective precipitation, ruthenium slag is prepared ruthenium trichloride in homemade reaction unit, has that technique is simple, energy consumption is low, ruthenium accumulation rate is high, impurity element is up to standard, distillation number of times is few, the reaction times is short, quality product is easily controlled, product yield high.
Accompanying drawing explanation
Fig. 1 is the production equipment schema of best mode for carrying out the invention.
Embodiment
Following examples are intended to the present invention to be further elaborated, rather than limitation of the present invention.Not departing under the prerequisite of national intellectual property protection, also may there be various changes and modifications, these changes and improvements all belong to the scope of protection of present invention.
Embodiment 1
Measure in the complicated Porcelain Jar that adds 500L containing ruthenium waste liquid 100Kg of lower concentration (ruthenium content is 9.53 ‰ by analysis), under stirring, slowly add one or both mixing acid in 5Kg hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, then add a kind of precipitation agent in 1906g ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, be diluted with water to 200L, unload still, conventional filtration, washing, the dry 1115g ruthenium slag (ruthenium content 84.29% by analysis) that obtains, in waste liquid, the yield of ruthenium is 98.62%.
Get 300g ruthenium slag and drop in reactor a, and to add 1.5L massfraction be 20 – 40% NaOH solution, in b and c, add 2L deionized water, to RuO
4in absorption bottle d, e, f, adding a kind of or two kinds of mixtures of the hydrochloric acid of 2.5L 2 – 10mol/L and methyl alcohol, ethanol, n-propyl alcohol, Virahol to keep massfractions is 0.01 – 6%, to adding 3L massfraction in tail gas absorption bottle g, is 15% NaOH solution.First open vacuum pump h, close purging valve i, check after the stopping property of whole preparation system, adjusting negative pressure is 0.08MPa.After feeding intake, heating a reactor, passes into chlorine after being warming up to 80 ℃, and controlling temperature of reaction is 105 ℃, and in reactor a, solution is brownish black, and produces a large amount of yellow RuO
4gas enters in absorption bottle d, e, f after removal of impurities bottle b and c, generates henna H
2ruC1
5solution, approximately reacts after 20min, and system reaction starts to slow down.Again add equivalent NaOH solution, continue to pass into chlorine, and produce yellow RuO
4gas, so repeat 2-3 time to reaction solution without reddish-brown till, after having reacted, slowly open blow-off valve i, close vacuum pump h, sucking-off H
2ruC1
5solution is concentrated through heating, crystallization, infrared drying obtain the crystallization of 673.12g ruthenium trichloride; Ruthenium trichloride quality meets HG/3679 – 2000 standards, RuCl after testing
3xH
2o crystallization ruthenium content is 36.95%, has good solubility property, ruthenium trichloride product yield 98.36%.
Embodiment 2
Measure in the complicated Porcelain Jar that adds 500L containing ruthenium waste liquid 200Kg of lower concentration (ruthenium content is 7.79 ‰ by analysis), under stirring, slowly add one or both mixing acid in 22Kg hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, then add a kind of precipitation agent in 4674g ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, be diluted with water to 400L, unload still, conventional filtration, washing, the dry 1797g ruthenium slag (ruthenium content 86.32% by analysis) that obtains, in waste liquid, the yield of ruthenium is 98.62%.
Get 300g ruthenium slag and drop in reactor a, and to add 1.8L massfraction be 30% NaOH solution, in b and c, add 2L deionized water, to RuO
4in absorption bottle d, e, f, adding a kind of or two kinds of mixtures of the hydrochloric acid of 2.5L 4mol/L and methyl alcohol, ethanol, n-propyl alcohol, Virahol to keep massfractions is 0.5%, to adding 3L massfraction in tail gas absorption bottle g, is 15% NaOH solution.First open vacuum pump h, close purging valve i, check after the stopping property of whole preparation system, adjusting negative pressure is 0.08MPa.After feeding intake, heating a reactor, passes into chlorine after being warming up to 80 ℃, and controlling temperature of reaction is 105 ℃, and in reactor a, solution is brownish black, and produces a large amount of yellow RuO
4gas enters in absorption bottle d, e, f after removal of impurities bottle b and c, generates henna H
2ruC1
5solution, approximately reacts after 20min, and system reaction starts to slow down.Again add equivalent NaOH solution, continue to pass into chlorine, and produce yellow RuO
4gas, so repeat 2-3 time to reaction solution without reddish-brown till, after having reacted, slowly open blow-off valve i, close vacuum pump h, sucking-off H
2ruC1
5solution is concentrated through heating, crystallization, infrared drying obtain the crystallization of 694.05g ruthenium trichloride; Ruthenium trichloride quality meets HG/3679 – 2000 standards, RuCl after testing
3xH
2o crystallization ruthenium content is 36.91%, has good solubility property, ruthenium trichloride product yield 98.92%.
Embodiment 3
Measure in the complicated Porcelain Jar that adds 500L containing ruthenium waste liquid 150Kg of lower concentration (ruthenium content is 1.06% by analysis), under stirring, slowly add one or both mixing acid in 18Kg hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, then add a kind of precipitation agent in 3975g ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, be diluted with water to 300L, unload still, conventional filtration, washing, the dry 1783g ruthenium slag (ruthenium content 88.39% by analysis) that obtains, in waste liquid, the yield of ruthenium is 99.12%.
Get 300g ruthenium slag and drop in reactor a, and to add 2L massfraction be 25% NaOH solution, to b, add 2.5L deionized water, to RuO
4in absorption bottle c, d, e, f, adding a kind of or two kinds of mixtures of the hydrochloric acid of 2.5L 4mol/L and methyl alcohol, ethanol, n-propyl alcohol, Virahol to keep massfractions is 0.5%, to adding 3L massfraction in tail gas absorption bottle g, is 15% NaOH solution.First open vacuum pump h, close purging valve i, check after the stopping property of whole preparation system, adjusting negative pressure is 0.08MPa.After feeding intake, heating a reactor, passes into chlorine after being warming up to 80 ℃, and controlling temperature of reaction is 105 ℃, and in reactor a, solution is brownish black, and produces a large amount of yellow RuO
4gas enters in absorption bottle d, e, f after removal of impurities bottle b and c, generates henna H
2ruC1
5solution, approximately reacts after 20min, and system reaction starts to slow down.Again add equivalent NaOH solution, continue to pass into chlorine, and produce yellow RuO
4gas, so repeat 2-3 time to reaction solution without reddish-brown till, after having reacted, slowly open blow-off valve i, close vacuum pump h, sucking-off H
2ruC1
5solution is concentrated through heating, crystallization, infrared drying obtain the crystallization of 707.19g ruthenium trichloride; Ruthenium trichloride quality meets HG/3679 – 2000 standards, RuCl after testing
3xH
2o crystallization ruthenium content is 37.02%, has good solubility property, ruthenium trichloride product yield 98.73%.
Embodiment 4
Measure in the complicated Porcelain Jar that adds 500L containing ruthenium waste liquid 250Kg of lower concentration (ruthenium content is 1.13% by analysis), under stirring, slowly add one or both mixing acid in 30Kg hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, then add a kind of precipitation agent in 5650g ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, be diluted with water to 450L, unload still, conventional filtration, washing, the dry 3112g ruthenium slag (ruthenium content 90.07% by analysis) that obtains, in waste liquid, the yield of ruthenium is 99.22%.2825 2802
Get 300g ruthenium slag and drop in reactor a, and to add 2L massfraction be 25% NaOH solution, to b, add 2.5L deionized water, to RuO
4in absorption bottle c, d, e, f, adding a kind of or two kinds of mixtures of the hydrochloric acid of 2.5L 6mol/L and methyl alcohol, ethanol, n-propyl alcohol, Virahol to keep massfractions is 1%, to adding 3L massfraction in tail gas absorption bottle g, is 15% NaOH solution.First open vacuum pump h, close purging valve i, check after the stopping property of whole preparation system, adjusting negative pressure is 0.08MPa.After feeding intake, heating a reactor, passes into chlorine after being warming up to 80 ℃, and controlling temperature of reaction is 105 ℃, and in reactor a, solution is brownish black, and produces a large amount of yellow RuO
4gas enters in absorption bottle d, e, f after removal of impurities bottle b and c, generates henna H
2ruC1
5solution, approximately reacts after 20min, and system reaction starts to slow down.Again add equivalent NaOH solution, continue to pass into chlorine, and produce yellow RuO
4gas, so repeat 2-3 time to reaction solution without reddish-brown till, after having reacted, slowly open blow-off valve i, close vacuum pump h, sucking-off H
2ruC1
5solution is concentrated through heating, crystallization, infrared drying obtain the crystallization of 721.85g ruthenium trichloride; Ruthenium trichloride quality meets HG/3679 – 2000 standards, RuCl after testing
3xH
2o crystallization ruthenium content is 36.89%, has good solubility property, ruthenium trichloride product yield 98.55%.
Claims (4)
1. the complicated method of preparing ruthenium trichloride containing ruthenium waste liquid of lower concentration, is characterized in that: lower concentration complicated containing ruthenium waste liquid through acidifying, the heavy ruthenium of selectivity, through the dry ruthenium slag that obtains enrichment of routine washing; Ruthenium slag adopts chlorine to add alkali distillation, absorption by Hydrochloric Acid, the concentrated ruthenium trichloride that is prepared into SILVER REAGENT that toasts.
2. lower concentration complexity as claimed in claim 1 is prepared the method for ruthenium trichloride containing ruthenium waste liquid, it is characterized in that, lower concentration is complicated is containing in ruthenium waste liquid, to add one or both mixing acid in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, the 1-15% that concentration is waste liquid to lower concentration is complicated containing the acidifying of ruthenium waste liquid.
3. lower concentration complexity as claimed in claim 1 is prepared the method for ruthenium trichloride containing ruthenium waste liquid, it is characterized in that, the heavy ruthenium of selectivity is a kind of precipitation agent adding in solution in ammonium sulfide, hydrazine hydrate, thiocarbamide, sodium borohydride, sodium hydroxide, the 1h that is heated to boil stops heating, 1 times of thin up, the consumption of precipitation agent is 0.5-10 times of ruthenium quality.
4. lower concentration as claimed in claim 1 is complicated prepares ruthenium trichloride containing ruthenium waste liquid, it is characterized in that, the ruthenium trichloride that ruthenium slag is prepared into SILVER REAGENT through chlorine distillation, absorption by Hydrochloric Acid, concentrated baking follows these steps to carry out:
1. under air-tight state negative pressure to add massfraction be the NaOH solution of 20-40%, the material proportion of thick ruthenium powder and sodium hydroxide solution is 1: 10 – 100;
2. be heated to 80 ℃, to step, pass into chlorine in 1., passing into chlorine flowrate is 50 – 120mL/min, controls temperature of reaction at 105 ℃, generates yellow RuO
4gas;
3. the RuO 2. step being generated
4gas is through deionized water purifying, passing into multistage absorption by Hydrochloric Acid liquid absorbs, concentration of hydrochloric acid is 2-10mol/L, temperature control is 25-40 ℃, in absorption by Hydrochloric Acid liquid, add reductive agent, reductive agent is a kind of or two kinds of mixtures of methyl alcohol, ethanol, n-propyl alcohol, Virahol, and the massfraction of reductive agent is 0.01 – 6%, and reaction generates red-brown H
2ruCl
5solution, tail gas passes into 15% NaOH solution absorption through negative pressure;
4. the H 3. step being generated
2ruCl
5, crystallization concentrated through conventional heating and infrared drying obtain the RuCl of chocolate
3crystal.
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Cited By (6)
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| CN106335932A (en) * | 2016-08-30 | 2017-01-18 | 昆明铂磊科技有限公司 | Production process of ruthenium trichloride |
| 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 |
| CN109136533A (en) * | 2018-10-19 | 2019-01-04 | 郴州高鑫铂业有限公司 | The method that quick separating extracts ruthenium from low content waste material containing ruthenium |
| CN110423896A (en) * | 2019-08-13 | 2019-11-08 | 江苏理工学院 | A method of ruthenium trichloride in recycling plating ruthenium waste liquid |
| CN115074537A (en) * | 2022-07-06 | 2022-09-20 | 山东海科创新研究院有限公司 | Ruthenium ion recovery method |
| CN115636445A (en) * | 2022-11-02 | 2023-01-24 | 金川集团股份有限公司 | Method for preparing high-purity ruthenium trichloride from low-concentration ruthenium-containing waste liquid |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106335932A (en) * | 2016-08-30 | 2017-01-18 | 昆明铂磊科技有限公司 | Production process of ruthenium trichloride |
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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 |
| CN109136533A (en) * | 2018-10-19 | 2019-01-04 | 郴州高鑫铂业有限公司 | The method that quick separating extracts ruthenium from low content waste material containing ruthenium |
| CN110423896A (en) * | 2019-08-13 | 2019-11-08 | 江苏理工学院 | A method of ruthenium trichloride in recycling plating ruthenium waste liquid |
| CN110423896B (en) * | 2019-08-13 | 2021-11-16 | 江苏理工学院 | Method for recovering ruthenium trichloride from ruthenium plating waste liquid |
| CN115074537A (en) * | 2022-07-06 | 2022-09-20 | 山东海科创新研究院有限公司 | Ruthenium ion recovery method |
| CN115636445A (en) * | 2022-11-02 | 2023-01-24 | 金川集团股份有限公司 | Method for preparing high-purity ruthenium trichloride from low-concentration ruthenium-containing waste liquid |
| CN115636445B (en) * | 2022-11-02 | 2024-04-12 | 金川集团股份有限公司 | Method for preparing high-purity ruthenium trichloride from low-concentration ruthenium-containing waste liquid |
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