CN115259248A - Preparation process of potassium osmate - Google Patents

Preparation process of potassium osmate Download PDF

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Publication number
CN115259248A
CN115259248A CN202210964458.3A CN202210964458A CN115259248A CN 115259248 A CN115259248 A CN 115259248A CN 202210964458 A CN202210964458 A CN 202210964458A CN 115259248 A CN115259248 A CN 115259248A
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CN
China
Prior art keywords
tube furnace
potassium hydroxide
osmate
absorption
drying
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Pending
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CN202210964458.3A
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Chinese (zh)
Inventor
苏临辉
苏林
赵彦杰
陈兴飞
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Yunnan Hongsheng Platinum New Material Technology Co ltd
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Yunnan Hongsheng Platinum New Material Technology Co ltd
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Priority to CN202210964458.3A priority Critical patent/CN115259248A/en
Publication of CN115259248A publication Critical patent/CN115259248A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G55/00Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum

Abstract

The present invention provides a preparation process of osmate potassium, and relates to the deep processing technology of noble metal, and the preparation process includes installing air filter in the outlet of the tube furnace, installing absorption system with potassium hydroxide solution in the other end of the tube furnace, connecting vacuum set to the absorption system to prepare osmate powder, potassium hydroxide solution and anhydrous ethanol for use, weighing osmate powder, pushing the weighed osmate powder into the tube furnace for heating, multistage absorption of the heated gaseous matter with the potassium hydroxide solution in the absorption system, adding ethanol into the absorption liquid until no purple red crystal is separated out, filtering, washing and drying to obtain osmate potassium.

Description

Preparation process of potassium osmate
Technical Field
The invention relates to the technical field of noble metal deep processing, in particular to a preparation process of potassium osmate.
Background
Osmium and its alloy are often regarded as the catalyst in synthetic ammonia or hydrogenation reaction, the catalytic effect is better, wherein osmium platinum alloy hardness is large, can make osmium platinum alloy scalpel in the pharmaceutical industry; the osmium tetroxide iridium alloy has extremely high melting point and hardness, is wear-resistant, can be used as a bearing of clocks and important instruments, and has long service life, osmium tetroxide is the most common compound of osmium and is generally used as a catalyst, an oxidant, a biological stain and the like, however, osmium tetroxide is volatile and has strong stimulation effect on eyes, noses and throats of human bodies, and a similar and safer osmium compound potassium osmate is required to replace the osmium tetroxide.
The new synthesis process of potassium osmate disclosed in Chinese patent No. CN106698530A includes the steps of pyrogenic process, water soaking, neutralization, filtering, washing, distillation, crystallization, etc. The present invention uses pure osmium powder as raw material, and adopts the pyrogenic smelting mode to make osmium be fed into solution, then adopts the steps of peroxide distillation and crystallization to obtain compound potassium osmate. The potassium osmate is powdery crystal at normal temperature, has stable property compared with osmium tetraoxide, is more convenient to store, transport and use, and overcomes the defects that less osmium compounds are commonly used in the prior art and the collection, packaging, storage and use of the osmium compounds are more troublesome.
In the above patent documents, osmium is put into solution by pyrometallurgy, and potassium osmate crystals are obtained by the steps of crystallization by peroxide distillation, etc. The method has large energy consumption in actual production, large sodium peroxide dosage and certain potential safety hazard, and is not beneficial to the actual preparation of potassium osmate.
Disclosure of Invention
Solves the technical problem
Aiming at the defects of the prior art, the invention provides a preparation process of potassium osmate, which solves the problems of large energy consumption, large reactant dosage and low potassium osmate yield in the prior art for preparing the potassium osmate.
Technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation process of potassium osmate, which is characterized in that: the preparation process comprises the following steps:
sp1: the equipment connection is characterized in that an air filter is additionally arranged at the outlet of the tube furnace, an absorption system with a potassium hydroxide solution is additionally arranged at the other end of the tube furnace, and a vacuum unit is connected with the absorption system to prepare osmium powder, the potassium hydroxide solution and absolute ethyl alcohol for later use;
sp2: osmium powder initial reaction, the osmium powder initial reaction is pushing the osmium powder into the tube furnace through a quartz boat in the tube furnace, and the tube furnace rapidly heats up to 200 ℃ and keeps the temperature for 1h after the osmium powder is pushed in, then slowly heats up to 400 ℃ and keeps the temperature for 2h, the gas generated by the reaction enters into the absorption system for absorption;
sp3: testing a product, namely when the output of osmium tetroxide is reduced by using thiourea at the end of the tube furnace, continuously heating to 600 ℃ for reaction for 30min;
sp4: extracting a product, wherein the extraction of the product is to cool the potassium hydroxide absorption liquid in the absorption system to room temperature, and slowly add absolute ethyl alcohol into the potassium hydroxide absorption liquid until no mauve crystal is separated out;
sp5: taking out the precipitated mauve crystal, washing the crystal to be neutral by using an ethanol solution with the mass fraction of 60%, and washing the crystal for 3 times by using absolute ethanol;
sp6: and drying and weighing, namely drying the washed crystal at 60 ℃ under vacuum condition to constant weight and weighing.
Preferably, the potassium hydroxide solution in the absorption system in the equipment connection is at least provided with five stages of systems for respective absorption, and the vacuum unit is connected with the end part of the final stage of potassium hydroxide solution.
Preferably, the drying and weighing are carried out by adopting an ultra-clean workbench surface, and the drying time is 50min.
Preferably, the pH value of the washed crystal is detected by a pH test paper in the treatment of the product, and the pH value range is 7 +/-0.5.
Preferably, the drying weighing is carried out by using a tray balance, and the judgment basis of the constant drying mass is that the difference value of the mass of the crystal in the adjacent three time periods is between 0.1 and 0.3, which indicates that the crystal is dried to the constant weight.
Advantageous effects
The invention provides a preparation process of potassium osmate. The method has the following beneficial effects:
weighing osmate powder, pushing the weighed osmate powder into a tube furnace through a quartz boat of the tube furnace, heating, performing multistage absorption on a gaseous substance generated by heating by using a potassium hydroxide solution in an absorption system, adding ethanol into the absorption solution until no purplish red crystal is separated out, and filtering, washing and drying to obtain the osmate.
Drawings
FIG. 1 is a diagram of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
as shown in fig. 1, a preparation process of potassium osmate, the specific preparation process is as follows:
sp1: the equipment is connected, wherein an air filter is additionally arranged at the outlet of the tube furnace, an absorption system with a potassium hydroxide solution is additionally arranged at the other end of the tube furnace, and a vacuum unit is connected with the absorption system to prepare osmium powder, the potassium hydroxide solution and absolute ethyl alcohol for later use;
sp2: osmium powder initial reaction, osmium powder initial reaction is pushing osmium powder into tube furnace through the quartz boat in the tube furnace, and the tube furnace after pushing osmium powder rapidly heating up to 200 ℃ and keeping warm for 1h, then slowly heating up to 400 ℃ and keeping warm for 2h, the gas generated by reaction enters into the absorption system for absorption;
sp3: checking the product, namely when the output of osmium tetroxide is reduced by using thiourea at the end of the tube furnace, continuously heating to 600 ℃ for reaction for 30min;
sp4: extracting a product, namely cooling the potassium hydroxide absorption liquid in the absorption system to room temperature, and slowly adding absolute ethyl alcohol into the potassium hydroxide absorption liquid until no mauve crystal is separated out;
sp5: treating the product, taking out the precipitated mauve crystal, washing the crystal to neutrality by using an ethanol solution with the mass fraction of 60%, and washing the crystal for 3 times by using absolute ethanol;
sp6: and drying and weighing, wherein the drying and weighing is to place the washed crystal under vacuum condition at 60 ℃ to dry to constant weight and then weigh.
The potassium hydroxide solution in the absorption system in the equipment connection is at least provided with five-stage system for absorption respectively, and the vacuum unit is connected with the end part of the last-stage potassium hydroxide solution, five-stage potassium hydroxide solution is arranged in the absorption system for absorbing the gas generated by osmate powder reaction in sequence, the absorption of the resultant can be more thorough through multi-stage absorption treatment, the phenomenon that the generated gas is discharged into the air to cause pollution due to incomplete absorption is prevented, the high yield of the osmate potassium is provided through complete absorption, the surface of an ultraclean workbench is used for drying when the drying weighing is carried out, the drying time is 50min, the PH value of the crystal after washing is detected by a PH test paper in the treatment of the resultant, the PH value ranges from 7 +/-0.5, the weighing is carried out by a tray balance in the drying weighing, the drying quality is constant according to the judgment that the mass difference value of the adjacent three time periods is between 0.1 and 0.3, the crystal is dried to the constant weight, the gas substance is pushed into a tube type heating furnace by utilizing the absorption system to absorb the potassium hydroxide solution, and the produced potassium hydroxide solution is filtered without much higher yield and the pollution is obtained through a red-free reaction by a multi-stage potassium hydroxide solution filtering method, thereby obtaining the potassium hydroxide solution without using less pollution-free potassium hydroxide solution.
The second embodiment is as follows:
the following results were obtained by performing the actual quantitative process of the reactants according to the above protocol, connecting the instrument, installing an air filter at the mouth of the tube furnace, installing a five-stage absorption system of potassium hydroxide solution behind the tube furnace, connecting the vacuum unit to the last stage absorption device, placing 50 g of osmium powder into the quartz boat, pushing into the tube furnace, rapidly heating the tube furnace to 200 ℃ and keeping the temperature for 1h, then slowly heating to 400 ℃ and keeping the temperature for 2h, when thiourea detected a decrease in osmium tetroxide production, continuing heating to 600 ℃ to react for 30min, cooling the potassium hydroxide absorption solution to room temperature, slowly adding absolute ethanol to the solution until no mauve crystal is precipitated, washing the crystal with 60% ethanol solution to neutrality, washing the crystal with absolute ethanol for 3 times, drying at 60 ℃ under vacuum to constant weight, and measuring to obtain 84.75 g of potassium osmate with a yield of 97.05%.
The third concrete embodiment:
the following results were obtained by performing the actual quantitative process of the reactants according to the above protocol, connecting the instrument, installing an air filter at the mouth of the tube furnace, installing a five-stage absorption system of potassium hydroxide solution behind the tube furnace, connecting the vacuum unit to the last stage absorption device, placing 80 g of osmium powder into a quartz boat, pushing into the tube furnace, rapidly heating the tube furnace to 200 ℃ and keeping the temperature for 1h, then slowly heating to 400 ℃ and keeping the temperature for 2h, when the thiourea detected a decrease in osmium tetroxide production, continuing heating to 600 ℃ to react for 30min, cooling the potassium hydroxide absorption solution to room temperature, slowly adding absolute ethanol to the solution until no mauve crystal is precipitated, washing the crystal with 60% ethanol solution to neutral, washing the crystal with absolute ethanol 3 times, drying at 60 ℃ under vacuum to constant weight, and measuring to obtain potassium osmate with a mass of 133.37 g and a yield of 95.40%.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a reference structure" does not exclude the presence of other identical elements in the process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. A preparation process of potassium osmate, which is characterized in that: the preparation process comprises the following steps:
sp1: the equipment connection is characterized in that an air filter is additionally arranged at the outlet of the tube furnace, an absorption system with a potassium hydroxide solution is additionally arranged at the other end of the tube furnace, and a vacuum unit is connected with the absorption system to prepare osmium powder, the potassium hydroxide solution and absolute ethyl alcohol for later use;
sp2: an osmium powder initial reaction, wherein the osmium powder initial reaction is that the osmium powder is pushed into the tube furnace through a quartz boat in the tube furnace, the tube furnace quickly heats up to 200 ℃ and keeps warm for 1h after the osmium powder is pushed in, then slowly heats up to 400 ℃ and keeps warm for 2h, and the gas generated by the reaction enters the absorption system for absorption;
sp3: testing a product, namely when the output of osmium tetroxide is reduced by using thiourea at the end of the tube furnace, continuously heating to 600 ℃ for reaction for 30min;
sp4: extracting a product, wherein the extraction of the product is to cool the potassium hydroxide absorption liquid in the absorption system to room temperature, and slowly add absolute ethyl alcohol into the potassium hydroxide absorption liquid until no mauve crystal is separated out;
sp5: taking out the precipitated mauve crystal, washing the crystal to neutrality by using an ethanol solution with the mass fraction of 60%, and washing the crystal 3 times by using absolute ethanol;
sp6: and drying and weighing, wherein the drying and weighing is to place the washed crystal under vacuum condition at 60 ℃ to dry to constant weight and then weigh.
2. The process of claim 1, wherein the potassium osmate is prepared by the following steps: the potassium hydroxide solution in the absorption system in the equipment connection is at least provided with five-stage systems for absorption respectively, and the vacuum unit is connected with the end part of the final stage of potassium hydroxide solution.
3. The process of claim 1, wherein the potassium osmate is prepared by the following steps: and drying the surface of an ultra-clean workbench during drying and weighing, wherein the drying time is 50min.
4. The process of claim 1, wherein the potassium osmate is prepared by the following steps: and in the treatment of the product, a PH test paper is used for detecting the PH value of the washed crystal, and the PH value range is 7 +/-0.5.
5. The process of claim 1, wherein the potassium osmate is prepared by the following steps: in the drying and weighing process, a tray balance is used for weighing, and the judgment basis of constant drying mass is that the mass difference value of the crystals in the adjacent three time periods is between 0.1 and 0.3, which indicates that the crystals are dried to constant weight.
CN202210964458.3A 2022-08-11 2022-08-11 Preparation process of potassium osmate Pending CN115259248A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2044084C1 (en) * 1993-06-15 1995-09-20 Комбинат "Североникель" Российского государственного концерна по производству цветных и драгоценных металлов "Норильский никель" Osmium-containing products processing method
CN1749421A (en) * 2005-09-01 2006-03-22 徐致钢 Process for extracting platinum metals from ore containing platinum metal
US20130108525A1 (en) * 2011-08-03 2013-05-02 The Curators Of The University Of Missouri Method for separation of chemically pure os from metal mixtures
RU2530188C1 (en) * 2013-09-05 2014-10-10 Открытое акционерное общество "Красноярский завод цветных металлов имени В.Н. Гулидова" (ОАО "Красцветмет") Method of producing osmium tetraoxide
CN106222438A (en) * 2016-08-29 2016-12-14 金川集团股份有限公司 A kind of from containing the method extracting osmium osmium material
CN106698530A (en) * 2017-02-28 2017-05-24 南京东锐铂业有限公司 Production process of potassium osmate
CN109055738A (en) * 2018-08-27 2018-12-21 浙江特力再生资源有限公司 Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine
CN109195920A (en) * 2016-07-06 2019-01-11 检验盖有限公司 Radiation source for inner cavity imaging capsule

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2044084C1 (en) * 1993-06-15 1995-09-20 Комбинат "Североникель" Российского государственного концерна по производству цветных и драгоценных металлов "Норильский никель" Osmium-containing products processing method
CN1749421A (en) * 2005-09-01 2006-03-22 徐致钢 Process for extracting platinum metals from ore containing platinum metal
US20130108525A1 (en) * 2011-08-03 2013-05-02 The Curators Of The University Of Missouri Method for separation of chemically pure os from metal mixtures
RU2530188C1 (en) * 2013-09-05 2014-10-10 Открытое акционерное общество "Красноярский завод цветных металлов имени В.Н. Гулидова" (ОАО "Красцветмет") Method of producing osmium tetraoxide
CN109195920A (en) * 2016-07-06 2019-01-11 检验盖有限公司 Radiation source for inner cavity imaging capsule
CN106222438A (en) * 2016-08-29 2016-12-14 金川集团股份有限公司 A kind of from containing the method extracting osmium osmium material
CN106698530A (en) * 2017-02-28 2017-05-24 南京东锐铂业有限公司 Production process of potassium osmate
CN109055738A (en) * 2018-08-27 2018-12-21 浙江特力再生资源有限公司 Noble metal recoverying and utilizing method in a kind of osmium iridium ruthenium mine

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Inventor after: Su Linhui

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