CN104773743A - Hydrothermal preparation method of editpotassium cyanide solution - Google Patents
Hydrothermal preparation method of editpotassium cyanide solution Download PDFInfo
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- CN104773743A CN104773743A CN201510169625.5A CN201510169625A CN104773743A CN 104773743 A CN104773743 A CN 104773743A CN 201510169625 A CN201510169625 A CN 201510169625A CN 104773743 A CN104773743 A CN 104773743A
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Abstract
The invention provides a hydrothermal preparation method of an editpotassium cyanide solution. According to the hydrothermal preparation method, potassium ferricyanide is used as a raw material. The hydrothermal preparation method comprises the steps of dissolution, hydrothermal reaction and separation of all units. The hydrothermal preparation method is characterized in that a K3Fe(CN)6 aqueous solution is put in a polytetrafluoroethylene lining of a hydrothermal kettle, after the hydrothermal kettle is sealed, the hydrothermal kettle is subjected to heat preservation for 24-72 hours at the temperature of 140-250 DEG C, after hydrothermal reaction, KOH solids, the amount of substance of which is three times as much as that of the K3Fe(CN)6, are added to the solution, after the KOH solids are dissolved by stirring, Fe2O3 precipitates are filtered out, and finally the KCN solution with corresponding concentration is obtained. By adopting the hydrothermal preparation method, equipment and technological processes can be simplified, and the cost is greatly reduced.
Description
One, technical field
The present invention relates to a kind of preparation method of inorganics, specifically a kind of hydrothermal preparing process of potassium cyanide solution.
Two, background technology
Potassium cyanide is soluble in water, has severe toxicity.Industrial for ore floatation extraction gold and silver, plating, the thermal treatment of iron and steel, organic nitrile manufacture.In addition, also for photograph, etching, lithographic printing etc.Usually in ammonia flow, be total to heat by salt of wormwood and carbon or obtained by calcium cyanamide and potassium hydroxide congruent melting, temperature required height, severe reaction conditions.Also have in enterprise and adopt ammonia sodium method (Chinese Patent Application No.: CN201010190367), cyanide melt method (Chinese Patent Application No.: CN201010190451) and light oil cracking (Chinese Patent Application No.: CN201010190313) to prepare, these method costs are all higher, and apparatus and process is complicated.
Three, summary of the invention
The present invention is intended to prepare potassium cyanide (KCN) by relatively simple technique, and technical problem to be solved simplifies existing technological process and processing condition.
This preparation method is with the Tripotassium iron hexacyanide (K
3fe (CN)
6) be raw material, comprise dissolving, hydro-thermal reaction and be separated each unit process, described dissolving is exactly by formation solution soluble in water for the Tripotassium iron hexacyanide, described hydro-thermal reaction is exactly polytetrafluoroethyllining lining potassium ferricyanide solution being placed in water heating kettle, 140 ~ 250 DEG C of insulations 24 ~ 72 hours after water heating kettle sealing, hydro-thermal reaction terminates to add the KOH solid being three times in solute Tripotassium iron hexacyanide molar weight in backward reaction solution, is separated after stirring and dissolving, namely filters Fe (OH)
3precipitation, finally obtains the potassium cyanide solution of respective concentration.So-called respective concentration be exactly under the condition reacted completely six times to the concentration of potassium ferricyanide solution concentration.
At room temperature, the complex ability of cryanide ion is extremely strong, therefore K
3fe (CN)
6solution can't be hydrolyzed and generate Fe (OH)
3precipitation, and along with temperature increase, the complex ability of cryanide ion sharply declines, now Fe
3+will OH preferentially and in the aqueous solution
-in conjunction with formation Fe (OH)
3, continue to be decomposed to form stable Fe
2o
3precipitation, after reacting completely, HCN and KCN only containing equimolar amount in remaining solution, after adding KOH and HCN neutralization reaction, only containing KCN in solution.Hydro-thermal reaction whether completely, directly have influence on the purity of final KCN solution, can Fe be passed through
2o
3the amount of precipitation estimates content and the purity of KCN solution indirectly, controls the reaction times.
K
3fe (CN)
6concentration higher than 1M time, under room temperature be difficult to completely dissolve (solubleness that Tripotassium iron hexacyanide molecular weight is 329,10 DEG C is 38g); Because cryanide ion complex ability is extremely strong, so solution directly can not be contacted with metal vessel, hydrothermal reaction kettle should with polytetrafluoroethyllining lining; When hydrothermal temperature is lower than 140 DEG C, hydro-thermal reaction speed is slow, even can not react, the Fe (OH) of generation
3also be difficult to be decomposed to form stable Fe
2o
3precipitation, when hydrothermal temperature is higher than 250 DEG C, production cost increases, and the easy temperature distortion of polytetrafluoroethyllining lining.
Obtain solid K CN only its solution to be dehydrated by known method, granulation.
Present method is also applicable to be that raw material prepares sodium cyanide solution or solid sodium cyanide with the Trisodium hexacyanoferrate.
This prepares the method for potassium cyanide solution, desired raw material K
3fe (CN)
6low price, purity is high, and equipment and process is simple, temperature required low, and therefore production cost is significantly less than the method adopted at present; And in whole reaction process, under solution is in alkaline condition, the HCN gas of severe toxicity is not volatile, and security is good always.
Four, embodiment
Embodiment 1:140 DEG C of hydro-thermal prepares 0.006M KCN solution
Be the K of 0.001M by concentration
3fe (CN)
6the aqueous solution is placed in the polytetrafluoroethyllining lining of water heating kettle, 140 DEG C of insulations 72 hours after water heating kettle sealing, adds in the solution and be three times in K after hydro-thermal reaction
3fe (CN)
6the KOH solid of amount of substance, filters out Fe after stirring and dissolving
2o
3precipitation, the solution finally obtained is the KCN solution that concentration is 0.006M.
Embodiment 2:180 DEG C of hydro-thermal prepares 0.06M KCN solution
Be the K of 0.01M by concentration
3fe (CN)
6the aqueous solution is placed in the polytetrafluoroethyllining lining of water heating kettle, 180 DEG C of insulations 48 hours after water heating kettle sealing, adds in the solution and be three times in K after hydro-thermal reaction
3fe (CN)
6the KOH solid of amount of substance, filters out Fe after stirring and dissolving
2o
3precipitation, the solution finally obtained is the KCN solution that concentration is 0.06M.
Embodiment 3:250 DEG C of hydro-thermal prepares 6M KCN solution
Be the K of 1M by concentration
3fe (CN)
6the aqueous solution is placed in the polytetrafluoroethyllining lining of water heating kettle, 250 DEG C of insulations 24 hours after water heating kettle sealing, adds in the solution and be three times in K after hydro-thermal reaction
3fe (CN)
6the KOH solid of amount of substance, filters out Fe after stirring and dissolving
2o
3precipitation, the solution finally obtained is the KCN solution that concentration is 6M.
Claims (1)
1. the hydrothermal preparing process of a potassium cyanide solution, take the Tripotassium iron hexacyanide as raw material, comprise dissolving, hydro-thermal reaction and be separated each unit process, it is characterized in that: polytetrafluoroethyllining lining iron cyanogen China potassium solution being placed in water heating kettle, 140 ~ 250 DEG C of insulations 24 ~ 72 hours after water heating kettle sealing, hydro-thermal reaction terminates to add the KOH solid being three times in solute Tripotassium iron hexacyanide molar weight in backward reaction solution, filters out Fe after stirring and dissolving
2o
3precipitation, finally obtains the potassium cyanide solution of respective concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510169625.5A CN104773743A (en) | 2015-04-10 | 2015-04-10 | Hydrothermal preparation method of editpotassium cyanide solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510169625.5A CN104773743A (en) | 2015-04-10 | 2015-04-10 | Hydrothermal preparation method of editpotassium cyanide solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104773743A true CN104773743A (en) | 2015-07-15 |
Family
ID=53615562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510169625.5A Pending CN104773743A (en) | 2015-04-10 | 2015-04-10 | Hydrothermal preparation method of editpotassium cyanide solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104773743A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911802A (en) * | 2006-09-05 | 2007-02-14 | 黎明化工研究院 | Preparation technology of water soluble metal cyanide salt |
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
| CN101955200A (en) * | 2010-05-27 | 2011-01-26 | 汪晋强 | Method for preparing potassium cyanide co-production mixed sulfate by using ammonia sodium residues |
-
2015
- 2015-04-10 CN CN201510169625.5A patent/CN104773743A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911802A (en) * | 2006-09-05 | 2007-02-14 | 黎明化工研究院 | Preparation technology of water soluble metal cyanide salt |
| CN101955200A (en) * | 2010-05-27 | 2011-01-26 | 汪晋强 | Method for preparing potassium cyanide co-production mixed sulfate by using ammonia sodium residues |
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 焦华等: "Fe3O4八面体微晶的水热法制备与表征", 《化学学报》 * |
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Application publication date: 20150715 |
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| RJ01 | Rejection of invention patent application after publication |