CN109811139B - Method for efficiently preparing environment-friendly gold leaching agent - Google Patents
Method for efficiently preparing environment-friendly gold leaching agent Download PDFInfo
- Publication number
- CN109811139B CN109811139B CN201910172027.1A CN201910172027A CN109811139B CN 109811139 B CN109811139 B CN 109811139B CN 201910172027 A CN201910172027 A CN 201910172027A CN 109811139 B CN109811139 B CN 109811139B
- Authority
- CN
- China
- Prior art keywords
- salen
- gold leaching
- leaching agent
- environment
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a heightMethod for efficiently preparing environment-friendly gold leaching agent, Salen-Na and FeCl3/Fe(NO3)3And (3) reacting to generate a high-efficiency catalyst Salen-Fe (III), uniformly mixing sodium cyanate, Salen-Fe (III) and a proper amount of pH regulator, reacting at 300-500 ℃, and cooling to normal temperature to obtain the environment-friendly gold leaching agent. The novel Salen-Fe (III) catalyst prepared by the invention efficiently catalyzes the preparation of the environment-friendly gold leaching agent, and reduces the activation energy of the reaction, so that the temperature required by the reaction is lower, and the energy consumption is saved; the environment-friendly gold leaching agent has good gold leaching effect, no toxicity, no pollution, environmental protection and safety.
Description
Technical Field
The invention relates to the technical field of mining and metallurgy engineering, in particular to a method for efficiently preparing an environment-friendly gold leaching agent.
Background
With the increasing importance of gold production and the diversification of resources in China, the gold leaching technology and the corresponding gold leaching agent are continuously developed, but the dominant gold leaching agent is still cyanide. However, cyanide has poor gold leaching effect on refractory gold ores containing C, As, Sb, Cu and the like, and has high toxicity and serious harm to the environment and human health. Therefore, the search for a high-efficiency, cyanide-free and environment-friendly gold leaching agent has become the focus of research in the field.
At present, most studied non-cyanide gold leaching agents mainly comprise thiourea, thiosulfate, lime-sulfur mixture and the like, but the non-cyanide gold leaching agents cannot be popularized and applied due to the defects of the non-cyanide gold leaching agents. In addition, in a novel environment-friendly gold leaching agent, the invention patent CN 201010553418.7 discloses a preparation method of a mineral separation additive, which is prepared by adopting inorganic substances (including urea, sodium hexametaphosphate, sodium sulfide, sodium bromide, sodium ferrocyanide, sodium carbonate and caustic soda) as raw materials and carrying out high-temperature reaction. The product has good gold leaching effect, does not contain highly toxic compounds, but has complex components of synthetic raw materials, and can generate complex chemical side reactions among various raw materials in the reaction process, thereby influencing the purity and the leaching effect of the product. The invention patent CN 201410210726.8 discloses a method for preparing a gold leaching agent by using urea, alkali and iron salt as raw materials and condensing at a high temperature of 600-900 ℃ under the action of an inhibitor and a catalyst. The gold leaching agent is suitable for heap leaching, tank leaching and carbon leaching processes of micro-fine gold ores, catalysts used for preparing the gold leaching agent are sodium chloride, ammonium chloride, calcium chloride and nickel chloride, and the reaction activity of the catalysts is insufficient, so that the reaction temperature is too high and the reaction conditions are harsh, and therefore, a class of catalysts for efficiently preparing the environment-friendly gold leaching agent is urgently needed to be developed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for efficiently preparing an environment-friendly gold leaching agent, which can reduce the activation energy of the reaction, thereby reducing the temperature required by the reaction and reducing the types of raw materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for efficiently preparing an environment-friendly gold leaching agent comprises the following steps:
s1Salen-Na and FeCl3Or Fe (NO)3)3Carrying out substitution reaction after mixing in a first solvent to obtain a Salen-Fe (III) catalyst; wherein, Salen-Na and FeCl3Or Fe (NO)3)3The weight ratio of (1): 0.5 to 1; the substitution reaction is carried out under the conditions that the temperature is 20-60 ℃ and the reaction time is 0.5-2 h;
s2, uniformly mixing the Salen-Fe (III) catalyst, the pH regulator and sodium cyanate, reacting for 0.2-1.5 h at 300-500 ℃, and cooling to normal temperature to obtain the environment-friendly gold leaching agent; wherein the Salen-Fe (III) catalyst, the pH regulator and the sodium cyanate are respectively 0.4-3 parts, 1-5 parts and 10-30 parts by mass.
The structural formula of Salen-Fe (III) is
X in the structural formula represents Cl or NO3. The Salen-Fe (III) is used as a catalyst for preparing the environment-friendly gold leaching agent, so that the activation energy of the reaction can be reduced, and the reaction rate can be accelerated. Can greatly reduce the reaction in the process of preparing the environment-friendly gold leaching agentAnd (3) temperature.
Further, in the step S1, the first solvent is an anhydrous aprotic solvent.
Still further, in step S2, the pH adjusting agent includes one or more of sodium carbonate, sodium bicarbonate, and sodium hydroxide.
Further, the preparation process of the Salen-Na comprises the following steps:
mixing the Salen ligand and the metal sodium in a second solvent to perform substitution reaction to obtain Salen-Na; wherein the weight ratio of the Salen ligand to the metal sodium is 5-8: 1; the substitution reaction is carried out at the temperature of 0-50 ℃ for 1-4 h.
The structural formula of Salen-Na is
Still further, the Salen ligand was prepared as follows:
mixing 1, 2-diphenyl-1, 2-ethylenediamine and salicylaldehyde, and then carrying out condensation reaction to obtain a Salen ligand; wherein the weight ratio of the 1, 2-diphenyl-1, 2-ethylenediamine to the salicylaldehyde is 1: 1.15-1.20; the condensation reaction is carried out at the temperature of 20-50 ℃ for 1-4 h. It should be noted that the structural formula of 1, 2-diphenyl-1, 2-ethylenediamine is
The structural formula of the Salen ligand is
Further, the second solvent is an aprotic solvent.
The invention has the beneficial technical effects that:
1. the novel Salen-Fe (III) catalyst prepared by the invention efficiently catalyzes the preparation of the environment-friendly gold leaching agent, and reduces the activation energy of the reaction, so that the temperature required by the reaction is lower, and the energy consumption is saved;
2. the environment-friendly gold leaching agent has good gold leaching effect, no toxicity, no pollution, environmental protection and safety;
3. the raw materials used in the invention are cheap and easily available, the process is simple, and the industrial production is easy to realize.
Drawings
FIG. 1 is a synthetic route diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the following examples are provided to illustrate the detailed embodiments and specific operations based on the technical solutions of the present invention, but the scope of the present invention is not limited to the examples.
Example 1
Weighing 52g of 1, 2-diphenyl-1, 2-ethylenediamine into a reaction vessel, adding 150mL of ethanol, stirring for dissolving, slowly adding 60g of salicylaldehyde into a mixed system, stirring for reacting for 1h at room temperature, filtering after the reaction is finished, and drying the obtained filter cake to obtain the Salen ligand.
40g of the Salen ligand is weighed in a reaction vessel, 100mL of anhydrous tetrahydrofuran is added and stirred to be dissolved, 7g of metallic sodium is slowly added into a mixed system, the mixture is stirred at room temperature for reaction for 2 hours, and then the tetrahydrofuran is removed by a rotary evaporator to obtain yellow Salen-Na solid with the yield of 95%.
24g of Salen-Na solid and 12g of ferric trichloride were weighed, 50mL of anhydrous tetrahydrofuran was added and dissolved with stirring, and the reaction was continued at 40 ℃ for 1 hour. After the reaction is finished, removing tetrahydrofuran by using a rotary evaporator to obtain a black solid, namely the Salen-Fe (III) catalyst. Oven drying, yield is 97%.
195.0g of sodium cyanate, 56.1g of sodium carbonate and 13.0g of Salen-Fe (III) catalyst are weighed, mixed and ground uniformly, then transferred into a muffle furnace to react for 0.5h at 400 ℃, and cooled to normal temperature to obtain the offwhite environment-friendly gold leaching agent with the yield of 90%.
Weighing 0.03g of gold leaching agent, dissolving the gold leaching agent in 100mL of water to obtain a colorless solution, adding 60g of gold-containing ore powder with the grade of 1.82g/t and the fineness of 0.0374mm accounting for 82%, stirring and leaching for 24h, filtering, washing tailings, measuring the gold content in the tailings by using atomic absorption, and calculating the leaching rate of gold to be 91.2%, which is higher than the leaching rate of sodium cyanide (89.1%) under the same conditions.
Example 2
The mass ratio of sodium cyanate, sodium carbonate and Salen-Fe (III) was 10:1:0.4, and the rest was the same as in example 1. The yield of the obtained environment-friendly gold leaching agent is 86%, and the leaching rate of gold is 78.5%.
Example 3
The mass ratio of sodium cyanate, sodium carbonate and Salen-Fe (iii) was 30:5:3, and the rest was the same as in example 1. The yield of the obtained environment-friendly gold leaching agent is 84%, and the leaching rate of gold is 90.6%.
Example 4
The reaction temperature in the muffle furnace was 300 ℃ and the other steps were the same as in example 1. The yield of the obtained environment-friendly gold leaching agent is 95%, and the leaching rate of gold is 82.5%.
Example 5
The reaction temperature in the muffle furnace was 500 ℃ and the other steps were the same as in example 1. The yield of the obtained environment-friendly gold leaching agent is 86%, and the leaching rate of gold is 89.6%.
Example 6
Weighing 52g of 1, 2-diphenyl-1, 2-ethylenediamine into a reaction vessel, adding 150mL of ethanol, stirring for dissolving, slowly adding 60g of salicylaldehyde into a mixed system, stirring for reacting for 1h at room temperature, filtering after the reaction is finished, and drying the obtained filter cake to obtain the Salen ligand.
40g of the Salen ligand is weighed in a reaction vessel, 100mL of anhydrous tetrahydrofuran is added and stirred to be dissolved, 7g of metallic sodium is slowly added into a mixed system, the mixture is stirred at room temperature for reaction for 2 hours, and then the tetrahydrofuran is removed by a rotary evaporator to obtain yellow Salen-Na solid with the yield of 95%.
50g of Salen-Na solid and 50g of ferric nitrate were weighed, 50mL of anhydrous tetrahydrofuran was added and dissolved with stirring, and the reaction was continued at 50 ℃ for 1 hour. After the reaction is finished, removing tetrahydrofuran by using a rotary evaporator to obtain a black solid, namely the Salen-Fe (III) catalyst. Oven drying, yield 94%.
195.0g of sodium cyanate, 21.5g of sodium hydroxide and 13.0g of Salen-Fe (III) catalyst are weighed, mixed, ground uniformly, transferred to a muffle furnace to react for 0.5h at 400 ℃, and cooled to normal temperature to obtain the off-white environment-friendly gold leaching agent with the yield of 93%.
Weighing 0.03g of gold leaching agent, dissolving the gold leaching agent in 100mL of water to obtain a colorless solution, adding 60g of gold-containing ore powder with the grade of 1.82g/t and the fineness of 0.0374mm accounting for 82%, stirring and leaching for 24h, filtering, washing tailings, measuring the gold content in the tailings by atomic absorption and calculating the leaching rate of gold to be 90.6%.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (4)
1. The method for efficiently preparing the environment-friendly gold leaching agent is characterized by comprising the following steps of:
s1Salen-Na and FeCl3Or Fe (NO)3)3Carrying out substitution reaction after mixing in a first solvent to obtain a Salen-Fe (III) catalyst; wherein, Salen-Na and FeCl3Or Fe (NO)3)3The weight ratio of (1): 0.5 to 1; the substitution reaction is carried out under the conditions that the temperature is 20-60 ℃ and the reaction time is 0.5-2 h;
the preparation process of the Salen-Na comprises the following steps:
mixing the Salen ligand and the metal sodium in a second solvent to perform substitution reaction to obtain Salen-Na; wherein the weight ratio of the Salen ligand to the metal sodium is 5-8: 1; the substitution reaction is carried out at the temperature of 0-50 ℃ for 1-4 h;
the Salen ligand was prepared as follows:
mixing 1, 2-diphenyl-1, 2-ethylenediamine and salicylaldehyde, and then carrying out condensation reaction to obtain a Salen ligand; wherein the weight ratio of the 1, 2-diphenyl-1, 2-ethylenediamine to the salicylaldehyde is 1: 1.15-1.20; the condensation reaction is carried out at the temperature of 20-50 ℃ for 1-4 h;
s2, uniformly mixing the Salen-Fe (III) catalyst, the pH regulator and sodium cyanate, reacting for 0.2-1.5 h at 300-500 ℃, and cooling to normal temperature to obtain the environment-friendly gold leaching agent; wherein the Salen-Fe (III) catalyst, the pH regulator and the sodium cyanate are respectively 0.4-3 parts, 1-5 parts and 10-30 parts by mass.
2. The method for efficiently preparing the environmentally friendly gold leaching agent according to claim 1, wherein in the step S1, the first solvent is an anhydrous aprotic solvent.
3. The method for efficiently preparing the environment-friendly gold leaching agent according to claim 1, wherein in the step S2, the pH adjusting agent comprises any one or more of sodium carbonate, sodium bicarbonate and sodium hydroxide.
4. The method for efficiently preparing the environment-friendly gold leaching agent according to claim 1, wherein the second solvent is an anhydrous aprotic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910172027.1A CN109811139B (en) | 2019-03-07 | 2019-03-07 | Method for efficiently preparing environment-friendly gold leaching agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910172027.1A CN109811139B (en) | 2019-03-07 | 2019-03-07 | Method for efficiently preparing environment-friendly gold leaching agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109811139A CN109811139A (en) | 2019-05-28 |
| CN109811139B true CN109811139B (en) | 2021-04-13 |
Family
ID=66608485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910172027.1A Active CN109811139B (en) | 2019-03-07 | 2019-03-07 | Method for efficiently preparing environment-friendly gold leaching agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109811139B (en) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2352650C2 (en) * | 2007-06-14 | 2009-04-20 | Владимир Алексеевич Гуров | Ecological method of complex extraction of nonferrous, rare and precious metals from ores and materials |
| CN102212085A (en) * | 2011-04-08 | 2011-10-12 | 河北工业大学 | Method for preparing Salen-metal complex |
| CN103695644A (en) * | 2013-12-13 | 2014-04-02 | 李敬坤 | Gold and silver leaching agent prepared from cyanate and method for recovering gold and silver by using leaching agent |
| CN103937986B (en) * | 2014-01-23 | 2016-08-24 | 柯柏友 | A kind of environment-friendly type noble metal selects the preparation method of agent |
| CN105950884A (en) * | 2016-04-27 | 2016-09-21 | 天津华勘矿业选冶技术开发有限公司 | Environmental-protection gold leaching agent and preparation method thereof |
| CN107475528A (en) * | 2017-08-23 | 2017-12-15 | 洛阳市鸿达科技有限公司 | A kind of environment-friendly type puies forward golden agent and its production technology |
-
2019
- 2019-03-07 CN CN201910172027.1A patent/CN109811139B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN109811139A (en) | 2019-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103981374B (en) | A kind of environmentally friendly cyanate soaks the synthetic method of golden agent | |
| CN102277483B (en) | Method for preparing rare earth chloride by using Baiyunebo rare earth concentrate | |
| CN101445446B (en) | Method for producing iron oxalate and by-products chrome metal and chromic acid | |
| CN106636667B (en) | A method of recycling manganese and silver from manganese-silver ore | |
| CN103805792B (en) | Special gold dissolving agent for gold ore | |
| CN106399712A (en) | Low-toxicity environment-friendly gold mineral separation agent and preparation method thereof | |
| CN101600809A (en) | The slurry preparation that use contains FeNi is used for the method for the raw material of stainless steel melt | |
| CN107475528A (en) | A kind of environment-friendly type puies forward golden agent and its production technology | |
| CN104232922A (en) | Sodium cyanate gold leaching technology | |
| CN113772693A (en) | Method for selectively leaching and extracting lithium from lithium iron phosphate waste | |
| CN109797290B (en) | Synthesis method of environment-friendly efficient gold leaching agent | |
| CN102795653B (en) | Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass | |
| CN102134099A (en) | Deep purification and phosphorus removal method for mixed liquor of coarse sodium tungstate solution and crystallized mother liquor | |
| CN105463203A (en) | Gold ore low-toxicity efficient mineral separation addition agent and preparing method thereof | |
| CN109811139B (en) | Method for efficiently preparing environment-friendly gold leaching agent | |
| CN101328540B (en) | Method for reclaiming sodium molybdate solution from molybdenum-containing leached residue | |
| CN103395825B (en) | A kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide | |
| CN112662887A (en) | Noble metal extracting and selecting agent | |
| CN108067216A (en) | The recovery method of base metal catalysts in a kind of catalytic coal gasifaction lime-ash | |
| CN101602702A (en) | The production technology of synthesizing thiourea by urea method | |
| CN103464305A (en) | Noble metals beneficiation agent and preparation method and application thereof | |
| CN100386450C (en) | Cooperated leaching method for low-grade intractable gold mine | |
| CN102051489A (en) | Method for recycling indium from acid pressure oxidative leaching liquid of zinc smelting product | |
| CN106636632B (en) | A kind of method that normal pressure decomposes wolframite or Scheelite-Wolframite Mixed Mine in alkaline system | |
| CN103898340B (en) | A kind of method utilizing nickel-molybdenum ore to prepare barium molybdate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhong Shuiping Inventor after: Li Guoyao Inventor after: Chen Hang Inventor after: Su Xiuzhu Inventor after: Wang June Inventor before: Chen Jinghe Inventor before: Zhong Shuiping Inventor before: Li Guoyao Inventor before: Chen Hang Inventor before: Su Xiuzhu Inventor before: Wang June |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |