CN107824340A - A kind of preparation method and application of noble metal collecting agent - Google Patents
A kind of preparation method and application of noble metal collecting agent Download PDFInfo
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- CN107824340A CN107824340A CN201711244275.XA CN201711244275A CN107824340A CN 107824340 A CN107824340 A CN 107824340A CN 201711244275 A CN201711244275 A CN 201711244275A CN 107824340 A CN107824340 A CN 107824340A
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- collecting agent
- noble metal
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- metal collecting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C329/00—Thiocarbonic acids; Halides, esters or anhydrides thereof
- C07C329/12—Dithiocarbonic acids; Derivatives thereof
- C07C329/14—Esters of dithiocarbonic acids
- C07C329/16—Esters of dithiocarbonic acids having sulfur atoms of dithiocarbonic groups bound to acyclic carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/02—Monothiocarbamic acids; Derivatives thereof
- C07C333/04—Monothiocarbamic acids; Derivatives thereof having nitrogen atoms of thiocarbamic groups bound to hydrogen atoms or to acyclic carbon atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/025—Precious metal ores
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of preparation method and application of noble metal collecting agent.The present invention is using industrial wastes fusel oil as raw material, after being dehydrated deodorization, add sodium hydroxide, after sodium hydroxide is completely dissolved, add carbon disulfide, material reaction completely and cool down after obtain liquid, then alkyl chloride reaction is added, monoethyl amine solution reaction is eventually adding, is separated, gained oil phase is precious metal ore collecting agent.The raw materials for production that the present invention uses are industrial wastes, source is wide, price is low, the noble metal collecting agent that processing and utilization is badly in need of into the major mine in China, both its pollution to environment can have been eliminated, it can turn waste into wealth simultaneously, reduce the production cost of noble metal collecting agent, improve the level of comprehensive utilization of Precious Metals mineral resources.
Description
Technical field
The present invention relates to beneficiation collecting agent technical field, particularly precious metal ore floating agent technical field, more specifically,
Be related to a kind of preparation method and application of noble metal collecting agent, suitable for associated gold silver ore flotation collector preparation method and
Using.
Background technology
Fusel oil is one of important pollution sources of the chemical industry waste waters such as wine brewing, sugaring, fermentation, be it is a kind of have it is special smelly
The colourless or faint yellow volatility oily liquids of taste and toxicity.Fusel oil is mainly more by isoamyl alcohol, isobutanol, octanol, ethanol etc.
Kind of alcohols and a small amount of organic acid, ketone, aldehyde and unsaturated organic compound composition, composition is extremely complicated, can be with by deep processing
Develop the tens of kinds of higher raw materials of industry of added value.It is but miscellaneous at present in view of complexity, stink and the toxicity of fusel oil ingredient
The comprehensive utilization of alcohol oil is confined to low-grade solvent, fuel and plastic plasticizer etc., and economic value is not high.
The purity of floating agent and the required precision of chemical reaction are strict not as other chemical products are extracted, as long as not
Containing harmful or have the composition of side effect, effect is not interfered with yet even if purity is not high.Main component is length in fusel oil
The alcohol not waited, additionally containing organic compounds such as a small amount of esters, ethers, ketone, terpenes, possesses prepare noble metal completely
The primary condition of beneficiation collecting agent.
At present, domestic and international noble metal collecting agent mainly includes esters, sulphur ammoniacum class, xanthate class, black powder class, ammonium class and answered
Dose out powders etc., more effectively include butyl ammonium aerofloat, P-60, aniline composite class, BK-301 etc., but factory in the industrial production
Family is mainly prepared using industrial chemicals, therefore production cost is of a relatively high.Although domestic major mine is to noble metal collecting
The demand of agent is very vigorous always, but is limited to higher medicament use cost, can only partly choose or use less.
In summary, fusel oil possesses prepare noble metal high selectivity completely as the industrial wastes containing a variety of alcohols
The material composition of collecting agent, a kind of method that noble metal collecting agent is prepared using fusel oil is developed, on the one hand can effectively reduce ring
Border pollution, turn waste into wealth, the floating agent on the one hand prepared can be applicable to bargh, improve gold and silver level of comprehensive utilization.
The content of the invention
The technical problem to be solved in the present invention is recycled and noble metal flotation collecting for existing industrial wastes fusel oil
The deficiency of agent technology, there is provided a kind of preparation method of noble metal collecting agent, using industrial wastes fusel oil as raw material, by simple easy
Capable step produces the flotation collector for having strong collecting performance to noble metals such as gold silver minerals.
Another technical problem to be solved by the present invention is that provide the noble metal collecting agent that the preparation method is prepared.
A present invention also technical problems to be solved are to provide the application of the noble metal collecting agent.
The purpose of the present invention is achieved by the following technical programs：
The present invention is off the beaten track, is conducted a research for the ethanol in fusel oil, extracts ethanol first, is prepared using the xanthate of maturation
Technique synthesizes ethyl xanthate, then proceedes to synthesize ethyl ammonia sulfate, a kind of strength collecting agent of noble metal is obtained, with existing copper-lead zinc
Conventional collecting agent butyl xanthate of sulphide ore etc. has basic difference substantially.
Specifically, using existing industrial wastes fusel oil as raw material, after being dehydrated deodorization, sodium hydroxide is added, treats hydroxide
After sodium is completely dissolved, add carbon disulfide, material reaction completely and cool down after obtain liquid, then add an alkyl chloride reaction,
Monoethyl amine solution reaction is eventually adding, is separated, gained oil phase is precious metal ore collecting agent.
Preferably, the sodium hydroxide uses fine powder, is gradually added under agitation.The sodium hydroxide fine powder is without tight
The granularity requirements of lattice, preferably cross 200 mesh sieve.
The addition carbon disulfide, being sufficiently stirred makes material reaction complete, and the liquid obtained after cooling is faint yellow.It is preferred that
Ground, the Adding Way of the monoethyl amine solution is to be slowly dropped into.
Preferably, the fusel oil（Molal weight is 46）, sodium hydroxide, carbon disulfide, an alkyl chloride, monoethyl amine it is anti-
It is 1 to answer mol ratio:1:1:1:1~3:2:1:1:1.
Preferably, fusel oil, sodium hydroxide, the total reaction time of carbon disulfide are no less than 30 minutes, reaction temperature control
Below 30 DEG C.
Preferably, the addition carbon disulfide, material reaction is complete and cools down, and is to be cooled to 25 DEG C of normal temperature.
Preferably, the time for adding alkyl chloride reaction is no less than 30 minutes, and reaction temperature is controlled at 40~50 DEG C.
Preferably, the time for adding monoethyl amine solution reaction is no less than 45 minutes, and reaction temperature is controlled at 15~50 DEG C.
Collecting agent is oil phase, is on whole solution, the separation can be extracted directly with separatory funnel, then be released
The solution of the latter half is i.e. separable.
Preferably, for the industrial wastes fusel oil as raw material, key component is ethanol, and its weight percent content is 40
~80%, other higher alcohols, ester and terpene compound are a little；Higher alcohol includes isoamyl alcohol, hexanol, octanol etc., and esters include caproic acid
Ethyl ester, cognac oil etc..According to the difference of ethanol content in raw material, ethyl ammonia sulfate content is varied from finished product, but raw material
More than 50% composition is ethyl ammonia sulfate in finished product under the conditions of middle ethanol weight percent content is 40~80%, you can reaches work
For the requirement of collecting agent.
Present invention simultaneously provides the noble metal collecting agent that the preparation method is prepared.
Present invention simultaneously provides application of the noble metal collecting agent in terms of noble metal flotation.
The present invention has the advantages that：
Although from alcohols synthesis xanthate technology in this area comparative maturity, traditional synthesis technique is with Chemical Manufacture
Alcohols be raw material, although material purity is high, cost is also higher.The raw materials for production that the present invention uses are industrial wastes, source
Extensively, price is low, the noble metal collecting agent that processing and utilization is badly in need of into the major mine in China, can both eliminate its pollution to environment,
It can turn waste into wealth simultaneously, reduce the production cost of noble metal collecting agent.
The present invention is off the beaten track, is conducted a research for the ethanol in fusel oil, extracts ethanol first, using the xanthate of maturation
Preparation technology synthesizes ethyl xanthate, then proceedes to synthesize ethyl ammonia sulfate, a kind of strength collecting agent of noble metal is obtained, with existing copper
Conventional collecting agent butyl xanthate of lead zinc sulphur ore etc. has basic difference substantially.
Final products of the present invention are ethyl ammonia sulfate, although in purity compared with chemical products synthesis ethyl ammonia sulfate content slightly
It is low, but the requirement of noble metal flotation collector is disclosure satisfy that, and cost of material is greatly reduced, acquired progress is in noble metal ore dressing
Field is extremely important, because reagent cost is always to restrict the main reason for mine is unwilling to use noble metal collecting agent.
The noble metal collecting agent being prepared using the inventive method, using the method for floating of routine, to associated gold silver ore
Thing has stronger selective collecting performance, while has frothing capacity concurrently, can effectively improve recovery of gold and silver.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of the present invention.
Embodiment
Embodiment 1
Fusel oil is derived from Guizhou liquor production factory, and through being dehydrated with after deodorization, measuring its component is：It is ethanol 62%, propyl alcohol 18%, different
Amylalcohol 8%, isobutanol 5%, water and other a small amount of organic compounds are 7%.Fusel oil samples 98g is weighed, is heated with constant water bath box
And temperature is controlled at 25 DEG C, use rotating speed to be stirred for 1200 revs/min of mechanical agitator, add sodium hydroxide fine powder 80g, treat molten
After solution is complete, carbon disulfide 76g is added, is stirred 1 hour, after material reaction is complete, an alkyl chloride 50g is added, stirs 45 points
Clock, industrial monoethyl amine solution 64mL is then slowly dropped into, stirred 1 hour, reactant is separated, and your gold gained oil phase is
Belong to mining collecting agent, component is mainly：（Second）Ethyl ammonia sulfate,（Isopropyl）Ethyl ammonia sulfate.It is through gas chromatography detection data
（Second）Ethyl ammonia sulfate content accounts for 70%.
Embodiment 2
Fusel oil is derived from Guangdong sugar refinery, and through being dehydrated with after deodorization, measuring its component is：Ethanol 75%, propyl alcohol 7%, isoamyl alcohol
5%th, isobutanol 5%, water and other a small amount of organic compounds are 8%.Fusel oil samples 75g is weighed, is heated and controlled with constant water bath box
Temperature processed uses rotating speed to be stirred for 1200 revs/min of mechanical agitator at 30 DEG C, adds sodium hydroxide fine powder 80g, to be dissolved complete
Quan Hou, carbon disulfide 76g is added, stirred 1 hour, after material reaction is complete, one alkyl chloride 50g of addition, stirring 45 minutes, so
After be slowly dropped into industrial monoethyl amine solution 64mL, stir 1 hour, reactant is separated, and gained oil phase is precious metal ore
With collecting agent, component is mainly：（Second）Ethyl ammonia sulfate.It is through gas chromatography detection data（Second）Ethyl ammonia sulfate content accounts for 82%.
Embodiment 3
Experimental study has been carried out to Area, Gejiu District, Yunnan Province card room argentiferous Copper Ores using noble metal collecting agent of the present invention.Raw ore is copper
Percentage composition 3.03%, silver-colored weight/mass percentage composition 21.77g/t are measured, copper mineral is mainly the copper sulfide mineral based on chalcopyrite,
Silver mineral is mainly the independent silver deposit thing such as native silver, acanthite, and collecting agent is done using the Z200 originally used, in ton ore deposit medicine
In the case of 4.5 yuan/ton of raw ores of agent cost, copper grade is obtained as the 23.92%, copper concentrate of the rate of recovery 97.10%, silver is in copper
In concentrate grade be 136g/t, the rate of recovery 70.25%.Using collecting agent of the present invention, reagent cost can be reduced to 3.5 yuan/
Ton raw ore, grade 23.56%, the copper concentrate of the rate of recovery 97.22% can be obtained, silver grade in copper concentrate is 152g/t, recovery
Rate is 77.05%, and silver-colored flotation effect is remarkably reinforced.
Embodiment 4
Carry out experimental study to Dali north government office in feudal China Copper Ores containing gold and silver using noble metal collecting agent of the present invention.Raw ore copper
Weight/mass percentage composition 0.70%, silver-colored weight/mass percentage composition 25.17g/t, golden weight/mass percentage composition 1.37g/t.Copper mineral predominantly with
Copper sulfide mineral based on chalcopyrite, but containing 15% or so combination cupric oxide, silver mineral is mainly acanthite, sulphur antimony
The independent silver deposit thing such as lead silver ore, vikingite, this matilidite, gold mineral are mainly the independent gold such as rusty gold, electrum
Mineral, collecting agent is done using original Z200, in the case of 4.0 yuan/ton of raw ores of ton ore deposit reagent cost, obtain copper grade
20.60%th, the copper concentrate of the rate of recovery 83.29%, gold and silver grade in copper concentrate are respectively 27.80g/t and 540.10g/t, are reclaimed
Rate is also respectively 50.05% and 62.13%.Using collecting agent of the present invention, reagent cost can be reduced to 3.2 yuan/ton of raw ores,
Can obtain copper grade 20.18%, the copper concentrate of the rate of recovery 83.95%, gold and silver grade in copper concentrate be respectively 26.15g/t and
525g/t, the rate of recovery are respectively increased to 59.05% and 69.15%, gold and silver flotation effect and are remarkably reinforced.
Claims (10)
1. a kind of preparation method of noble metal collecting agent, it is characterised in that be using industrial wastes fusel oil as raw material, removed through dehydration
After smelly, add sodium hydroxide, after sodium hydroxide is completely dissolved, add carbon disulfide, material reaction completely and cool down after obtain
Liquid, alkyl chloride reaction is then added, is eventually adding monoethyl amine solution reaction, is separated, gained oil phase is that precious metal ore is used
Collecting agent.
2. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that sodium hydroxide uses fine powder,
It is gradually added under stirring state；The Adding Way of the monoethyl amine solution is to be slowly dropped into.
3. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that the fusel oil, sodium hydroxide,
Carbon disulfide, an alkyl chloride, the reaction mol ratio of monoethyl amine are 1:1:1:1:1~3:2:1:1:1.
4. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that fusel oil, sodium hydroxide, two sulphur
The total reaction time for changing carbon is no less than 30 minutes, and reaction temperature is controlled below 30 DEG C.
5. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that add an alkyl chloride reaction when
Between be no less than 30 minutes, reaction temperature control at 40~50 DEG C.
6. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that add monoethyl amine solution reaction
Time is no less than 45 minutes, and reaction temperature is controlled at 15~50 DEG C.
7. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that in the industrial wastes fusel oil
The weight percent content of ethanol is 40~80%.
8. the preparation method of noble metal collecting agent according to claim 1, it is characterised in that the industrial wastes fusel oil comes
From in waste liquid caused by wine brewing, sugaring or fermenting and producing.
9. the noble metal collecting agent that a kind of any one of claim 1 to 8 preparation method is prepared.
10. application of the noble metal collecting agent in terms of noble metal flotation described in claim 9.
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| CN201711244275.XA CN107824340A (en) | 2017-11-30 | 2017-11-30 | A kind of preparation method and application of noble metal collecting agent |
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| CN201711244275.XA CN107824340A (en) | 2017-11-30 | 2017-11-30 | A kind of preparation method and application of noble metal collecting agent |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2691635A (en) * | 1953-05-20 | 1954-10-12 | Dow Chemical Co | Process for the manufacture of dialkyl thionocarbamates |
| CN101259451A (en) * | 2008-04-24 | 2008-09-10 | 中南大学 | Preparation of floating collector |
| CN101698160A (en) * | 2009-10-26 | 2010-04-28 | 中南大学 | Sulfide flotation collector and preparation method |
| CN102690218A (en) * | 2012-04-27 | 2012-09-26 | 中南大学 | Method for synthesizing xanthate |
| CN103817014A (en) * | 2014-02-21 | 2014-05-28 | 中南大学 | Preparation method for granular xanthate |
-
2017
- 2017-11-30 CN CN201711244275.XA patent/CN107824340A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2691635A (en) * | 1953-05-20 | 1954-10-12 | Dow Chemical Co | Process for the manufacture of dialkyl thionocarbamates |
| CN101259451A (en) * | 2008-04-24 | 2008-09-10 | 中南大学 | Preparation of floating collector |
| CN101698160A (en) * | 2009-10-26 | 2010-04-28 | 中南大学 | Sulfide flotation collector and preparation method |
| CN102690218A (en) * | 2012-04-27 | 2012-09-26 | 中南大学 | Method for synthesizing xanthate |
| CN103817014A (en) * | 2014-02-21 | 2014-05-28 | 中南大学 | Preparation method for granular xanthate |
Non-Patent Citations (1)
| Title |
|---|
| 谭鑫,钟宏,张永: "硫氨酯捕收剂的合成", 《铜业工程》 * |
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Application publication date: 20180323 |
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