CN109569894A - Quaternary ammonium salt ionic liquid cation-collecting agent and its preparation method and application - Google Patents
Quaternary ammonium salt ionic liquid cation-collecting agent and its preparation method and application Download PDFInfo
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- CN109569894A CN109569894A CN201811511382.9A CN201811511382A CN109569894A CN 109569894 A CN109569894 A CN 109569894A CN 201811511382 A CN201811511382 A CN 201811511382A CN 109569894 A CN109569894 A CN 109569894A
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- collecting agent
- quaternary ammonium
- ammonium salt
- ionic liquid
- salt ionic
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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
- B03D1/02—Froth-flotation processes
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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
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- 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
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to beneficiation reagents, more particularly to a kind of novel quaternary ammonium salt ionic liquid cation-collecting agent and preparation method thereof, it include following steps: under solvent existence condition, the cetyl trimethylammonium bromide of identical molar ratio is mixed with sodium salicylate solution, it is stirred to react under the conditions of 10-70 DEG C 5-20 hours, gained organic liquid carries out centrifuge washing, remaining liq is subjected to decompression rotary distillation under the conditions of 60-120 DEG C after washing, until solvent distillation is completely, target liq is obtained after being cooled to room temperature.Quaternary ammonium salt collecting agent provided by the invention has the advantage that 1) this medicament is easily soluble in water in configuration process compared with traditional cation collecting agent lauryl amine, and lauryl amine needs to be dissolved with acid-mixed conjunction, therefore medicament use is easier.2) this medicament synthetic route is simple and easy, and selectivity is good, and collecting performance is strong.3) it remains to obtain preferable flotation effect in the case where not adding inhibitor.
Description
Technical field
The present invention relates to beneficiation reagents, and in particular to a kind of novel quaternary ammonium salt ionic liquid cation-collecting agent and its preparation
Method.
Background technique
The iron ore deposit in China substantially belongs to poor iron ore, has the characteristics that the low high silicon of iron, gangue in magnetic iron ore and bloodstone
Mineral are mainly quartz.It is nothing with magnetic method if quartz and magnetic iron ore are existed in the form of intergrowth in magnetic iron ore
Method removes gangue, higher so as to cause content quartzy in concentrate.The benefit of blast furnace when higher quartz content can reduce smelting
With coefficient, so that the increased costs of ironmaking.Therefore, Counterfloatating desiliconization, mention iron drop it is miscellaneous, the fine iron breeze for providing high quality is very
It is necessary.Reverse floatation process has been used for industrial production from 1970s, proves through a large number of experiments and industrial production anti-floating
Choosing is a kind of method for mentioning Fe and reducing Si efficiently, economic.
Although traditional cationic surfactant performance is brilliant, most of to be more toxic, be difficult to biodegrade, Yi
It is absorbed and pollution of ecological environment in sewage treatment by sludge.And since cationic surfactant is using more and more, people
More worry that it is a large amount of using whether can cause environmental pollution, if having bio-toxicity and it is biodegradable the problems such as.
Therefore exploitation novel environment friendly functional surfactant by be cationic surfactant development trend.
And ionic liquid is in room temperature or closely under room temperature completely by organic cation and organic anion or inorganic yin
From the molecular molten salt system being in a liquid state.Compared to solid-state material, it is liquid;It is compared to traditional liquid material,
It is ion again.Therefore, ionic liquid has unique chemical property and physical property, such as extremely low vapour pressure and non-volatile
The features such as property, low melting point, high thermal stability, selective dissolution and designability.Ionic liquid becomes because of the above feature to be had concurrently
The unique material of liquid and solid function and characteristic.
In addition to this due to the designability of ionic liquid, the ionic liquid of needs is targetedly synthesized.Ionic liquid
Research the green chemistry chemical technology field Quick Extended since most to functional material, energy field.Although ionic liquid obtains
It is used to so extensive, but rarely has people to be applied in flotation field at present.Moreover, mineral processing in China industry flotation field is general
Store-through pollutes and high energy consumption issues in floating agent, perhaps replaces traditional floating agent, it can be achieved that tradition is floating with ionic liquid
The upgrading of choosing and great innovation.Therefore, ionic liquid is applied to flotation to the pollution of alleviation China's floating agent and tradition
The upgrading of floating agent is of great significance.
Summary of the invention
A kind of environmental-friendly the purpose of the present invention is synthesizing, high-efficiency low-toxicity, System of Flotation Reagent is simple, and to silicate-containing
The reverse flotation of class mineral has good collecting performance and selects the novel quaternary ammonium salt ionic liquid cation-collecting agent of performance, and mentions
For easy-operating medicament preparation method.
The technical solution adopted by the present invention to solve the technical problems is: quaternary ammonium salt ionic liquid cation-collecting agent,
Chemical formula are as follows:
The preparation method of quaternary ammonium salt ionic liquid cation-collecting agent provided by the invention, includes following steps: solvent
Under existence condition, the cetyl trimethylammonium bromide of identical molar ratio is mixed with sodium salicylate solution, in 10-70 DEG C of condition
Under be stirred to react 5-20 hours, gained organic liquid carry out centrifuge washing, after washing by remaining liq under the conditions of 60-120 DEG C
Decompression rotary distillation is carried out, until solvent distillation is completely, obtains target liq after being cooled to room temperature.
According to the above scheme, the solvent is chloroform, acetone, methanol, ether, benzene or ethyl alcohol.
According to the above scheme, the concentration of the sodium salicylate solution is 10%-60%g/L.
According to the above scheme, the molar ratio of the solvent and cetyl trimethylammonium bromide is (10~12.5): 1.
According to the above scheme, the centrifuge washing uses deionized water.
The present invention provides above-mentioned quaternary ammonium salt ionic liquid cation-collecting agent (cetyl trimethyl ammonium salicylate) and is used for
The application of the flotation collector of quartzy minal and magnetic iron ore minal mixed mineral.
The method that the medicament is used for minal flotation are as follows: with deionized water by novel ion liquid cation-collecting agent
It is configured to 0.0025 × 10-3Mol/L, 0.005 × 10-3Mol/L, 0.01 × 10-3Mol/L, 0.015 × 10-3Mol/L, 0.03 ×
10-3Mol/L, 0.06 × 10-3The solution of mol/L various concentration.It weighs 2.0g minal and is placed in II 5-35G hanging trough flotator of XFG
In 25ml flotation cell and to keep pulp density be 10%, mixing speed set at 25 DEG C of room temperature as 2000 revs/min, addition difference
The collecting agent of concentration stirs 2 minutes, is then 7 addition NaOH or HCl regulators by pH value and lowers in 2000 revs/min of revolving speed
Slurry 2 minutes, flotation 4 minutes.Product drying weighing in froth pulp and slot is calculated into the rate of recovery, it is final to determine the best of collecting agent
Concentration is 0.015 × 10-3mol/L.Later, carry out pH value condition experiment under the conditions of optium concentration, pH value is set to 3,5,
7,9,11, it can finally show that in concentration be 0.015 × 10-3The rate of recovery of quartz minal can reach 97% when mol/L, pH=7,
And the magnetic iron ore minal rate of recovery is almost 0%.
It is by the method that the medicament is used for artificial mixed ore flotation: weighs 2.0g minal, wherein quartz and magnetic iron ore
Ratio is 1:3.It is 0.015 × 10 in drug concentration-3Flotation is carried out when mol/L, pH=7, Iron grade is in gained concentrate
66.32%, the rate of recovery 98.30%.
Quaternary ammonium salt collecting agent provided by the invention has the advantage that compared with traditional cation collecting agent lauryl amine
1) this medicament is easily soluble in water in configuration process, and lauryl amine needs to be dissolved with acid-mixed conjunction, therefore medicament
Using easier.
2) this medicament synthetic route is simple and easy, and selectivity is good, and collecting performance is strong.
3) it remains to obtain preferable flotation effect in the case where not adding inhibitor.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of cetyl trimethyl ammonium salicylate ionic liquid.
Specific implementation method
The present invention is described in detail by the following examples, these embodiments are only preferably to explain the present invention, not as to this hair
Bright limitation.
Embodiment 1
In 100ml beaker, 20ml (0.25mol) chloroform is added as reaction dissolvent, is added 7.3g (0.02mol)
Cetyl trimethylammonium bromide and 30% bigcatkin willow mixed by 3.2g (0.02mol) sodium salicylate and deionized water
Acid sodium solution.Beaker is placed in magnetic stirring apparatus and is stirred 10 hours with (30 DEG C) of constant temperature, products therefrom is carried out with deionized water
Washing, products therefrom rotates distilling off solvent at 100 DEG C by Rotary Evaporators after washing, and obtaining weak yellow liquid is target
Product, infrared spectrogram are shown in Fig. 1.It can be seen that from collecting agent infrared spectrogram in 964cm-1、1462cm-1、1468cm-1Place is to catch
Receive the quaternary ammonium salt characteristic absorption peak of agent;In 2900cm-1Nearby there are three very strong absorption peak 2920cm-1、2870cm-1、
2850cm-1, this is the absorption peak for being saturated methyl, methylene, embodies the knot of chain alkyl methyl type cationic surfactant
Structure characteristic;700-760cm-1It is the absorption peak of the rocking vibration of the long-chain methylene of collecting agent M-M;Therefore, by infrared
Spectrum is it has been confirmed that synthesized product is target product quaternary ammonium salt ion liquid cation-collecting agent.
Synthetic product is used for minal flotation, the quartzy minal and magnetic iron ore minal for this invention are by Australia
Big Leah University of Queensland Julius Kruttschnitt Mineral Research Center provides, and chemical composition analysis is shown in Table 1 respectively,
Table 2.Ionic liquid is configured to 0.0025 × 10 using deionized water-3Mol/L, 0.005 × 10-3Mol/L, 0.01 × 10- 3Mol/L, 0.015 × 10-3Mol/L, 0.03 × 10-3Mol/L, 0.06 × 10-3The solution of mol/L various concentration.Weigh 2.0g
It is 10% that minal, which is placed in II 5-35G hanging trough flotator 25ml flotation cell of XFG and keeps pulp density, is divided at 25 DEG C of room temperature
Determine mixing speed be 2000 revs/min, be added various concentration collecting agent stir 2 minutes, then by pH value be 7 be added NaOH or
HCl regulator is sized mixing 2 minutes, after flotation in 4 minutes, product drying weighing in froth pulp and slot is calculated the rate of recovery, most
The optium concentration for determining collecting agent eventually is 0.015 × 10-3mol/L.Later, it is real that pH value condition is carried out under the conditions of optium concentration
It tests, pH value is set to 3,5,7,9,11, can get table 3,4 index of table.
Synthetic product is used for artificial mixed ore flotation, weighs 2.0g minal, wherein quartz is 1 with magnetic iron ore ratio:
3.It is 0.015 × 10 in drug concentration-3Flotation is carried out when mol/L, pH=7, obtains floatation indicators table 5.It can be seen that according to table 5,
Iron grade is 66.32% in concentrate, slightly below uses 68.88% when lauryl amine, but its rate of recovery is 98.30% much higher than making
65.81% when with lauryl amine.In the case where not using inhibitor, the separation performance of lauryl amine is obviously not so good as synthetic drug
Agent.
The quartzy chemical composition analysis result table (%) of table 1
2 magnetic iron ore chemical composition analysis result table (%) of table
Influence (mol/L) of the 3 collecting agent concentration of table to the minal rate of recovery
Influence of the table 4pH value to the minal rate of recovery
5 artificial mixed ore floatation indicators of table
Embodiment 2
In 100ml beaker, 20ml (0.25mol) chloroform is added as reaction dissolvent, is added 7.3g (0.02mol)
Cetyl trimethylammonium bromide and 50% bigcatkin willow mixed by 3.2g (0.02mol) sodium salicylate and deionized water
Acid sodium solution.Beaker is placed in magnetic stirring apparatus and is stirred 9 hours with 60 DEG C of constant temperature, products therefrom is washed with deionized water
It washs, products therefrom rotates distilling off solvent at 90 DEG C by Rotary Evaporators after washing, and obtaining weak yellow liquid is that target produces
Object.
Minal, which is carried out, by the method in embodiment 1 tests available table 6, table 7,8 index of table.
Influence (mol/L) of the 6 collecting agent concentration of table to the minal rate of recovery
Influence of 7 pH value of table to the minal rate of recovery
8 artificial mixed ore floatation indicators of table
Embodiment 3
In 100ml beaker, 20ml (0.25mol) chloroform is added as reaction dissolvent, is added 7.3g (0.02mol)
Cetyl trimethylammonium bromide and 60% bigcatkin willow mixed by 3.2g (0.02mol) sodium salicylate and deionized water
Acid sodium solution.Beaker is placed in magnetic stirring apparatus and is stirred 16 hours with 70 DEG C of constant temperature, products therefrom is washed with deionized water
It washs, products therefrom rotates distilling off solvent at 120 DEG C by Rotary Evaporators after washing, and obtaining weak yellow liquid is that target produces
Object.
Minal, which is carried out, by the method in embodiment 1 tests available table 9, table 10,11 index of table.
Influence (mol/L) of the 9 collecting agent concentration of table to the minal rate of recovery
Influence of 10 pH value of table to the minal rate of recovery
11 artificial mixed ore floatation indicators of table
Claims (7)
1. quaternary ammonium salt ionic liquid cation-collecting agent, chemical formula are as follows:
2. the preparation method of quaternary ammonium salt ionic liquid cation-collecting agent described in claim 1, includes following steps: solvent
Under existence condition, the cetyl trimethylammonium bromide of identical molar ratio is mixed with sodium salicylate solution, in 10-70 DEG C of condition
Under be stirred to react 5-20 hours, gained organic liquid carry out centrifuge washing, after washing by remaining liq under the conditions of 60-120 DEG C
Decompression rotary distillation is carried out, until solvent distillation is completely, obtains target liq after being cooled to room temperature.
3. the preparation method of quaternary ammonium salt ionic liquid cation-collecting agent as described in claim 2, it is characterised in that described
Solvent is chloroform, acetone, methanol, ether, benzene or ethyl alcohol.
4. the preparation method of quaternary ammonium salt ionic liquid cation-collecting agent as described in claim 2, it is characterised in that described
The concentration of sodium salicylate solution is 10%-60%g/L.
5. the preparation method of quaternary ammonium salt ionic liquid cation-collecting agent as described in claim 2, it is characterised in that described
The molar ratio of solvent and cetyl trimethylammonium bromide is (10~12.5): 1.
6. the preparation method of quaternary ammonium salt ionic liquid cation-collecting agent as described in claim 2, it is characterised in that described
Centrifuge washing uses deionized water.
7. quaternary ammonium salt ionic liquid cation-collecting agent described in claim 1 is used for quartzy minal and magnetic iron ore minal is mixed
Close the application of the flotation collector of mineral.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111185307A (en) * | 2020-01-13 | 2020-05-22 | 南昌航空大学 | Application of gemini quaternary ammonium salt collecting agent |
CN112495589A (en) * | 2020-11-06 | 2021-03-16 | 武汉理工大学 | Eutectic solvent cation collecting agent and preparation method and application thereof |
CN113680534A (en) * | 2021-08-30 | 2021-11-23 | 东北大学 | Fine-particle iron mineral collecting agent and coarse-fine asynchronous flotation method for carbonate-containing iron ore |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111185307A (en) * | 2020-01-13 | 2020-05-22 | 南昌航空大学 | Application of gemini quaternary ammonium salt collecting agent |
CN112495589A (en) * | 2020-11-06 | 2021-03-16 | 武汉理工大学 | Eutectic solvent cation collecting agent and preparation method and application thereof |
CN113680534A (en) * | 2021-08-30 | 2021-11-23 | 东北大学 | Fine-particle iron mineral collecting agent and coarse-fine asynchronous flotation method for carbonate-containing iron ore |
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Application publication date: 20190405 |