CN103712838B - A kind of Collophanite flotation anionic collector detects pre-treating method - Google Patents
A kind of Collophanite flotation anionic collector detects pre-treating method Download PDFInfo
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- CN103712838B CN103712838B CN201310749813.6A CN201310749813A CN103712838B CN 103712838 B CN103712838 B CN 103712838B CN 201310749813 A CN201310749813 A CN 201310749813A CN 103712838 B CN103712838 B CN 103712838B
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Abstract
The present invention relates to a kind of method that phosphate rock floating anionic collector detects pre-treatment, belong to collophanite flotation treatment method.Main following processing step: a. that contains gets 10g flotation phosphate ore anionic collector, puts into teflon counteracting tank, adds 30 ~ 35mL distilled water, regulates solution to pH=2, then adds same dilution heat of sulfuric acid 3mL, cover helixseal lid with dilute sulfuric acid; B. put into micro-wave oven, effect 10min, takes out and leaves standstill 2 ~ 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL; C. a large amount of hot distilled water washing, is washed till solution ph 6.8 ~ 7, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.Teflon counteracting tank described in step a is FR-50 type; Regulate aqueous solution to be measure the commercially available AR level concentrated sulphuric acid to add same volume distilled water formulated with dilute sulfuric acid, the volume ratio of the concentrated sulphuric acid and distilled water is 1:1; Adding dilution heat of sulfuric acid consistent with adjustment dilute sulfuric acid concentration, is same solution; PH=2 accurate pH test paper or pH meter detect and draw.
Description
Technical field
The present invention relates to a kind of method that phosphate rock floating anionic collector detects pre-treatment.Belong to collophanite flotation treatment method.
Background technology
In minerals processing industry, flotation to be separated in phosphorus ore the most effective method of valuable mineral and gangue mineral and technology, what play a crucial role in flotation is flotation collector, add the flotation collector that collecting power is strong, valuable mineral can be adsorbed on collecting agent surface and form surface hydrophobicity film, this hydrophobic membrane forms foam and also takes valuable mineral out of collophanite system, thus realizes being separated of valuable mineral and gangue mineral.At present with regard to phosphate rock floating, in phosphate rock floating with comparatively generally anion collecting agent, the product of commercial anionic type collecting agent is many, some soaps, the derivant of fatty acid, the modifier etc. of fatty acid, the starting material of anion collecting agent, synthesis, research and development, use the composition waiting and all require to know wherein, reach the object precisely used, how quick, analyze accurately and seem particularly important, along with the fast development of China's Phosphate Fertilizer Industry, the demand of phosphorus concentrate is also increased every year, and high-quality phosphate rock resource has been developed almost, therefore be faced with to process low-grade, the huge difficult problem of the raw ore that associated minerals are many, develop these ore deposits inferior, flotation technology is a technology crucial especially, so stable floating agent of carrying out fast is analyzed pre-treatment and is had larger realistic meaning.Tradition pre-treating method is in sour environment (pH is less than 2), agitating heating 60min under unlatching ventilation equipment, and a large amount of hot water wash is to neutral afterwards, draws out fatty acid to be measured.(can be regarded as the reversed reaction of fatty acid saponification reaction), complex operation is consuming time, smells taste large.Now utilize microwave that chemical substance is reacted, its reaction velocity comparatively conventional heating methods fast ten times and even thousand times, provide a kind of can be simple and quick, stable, and anionic collector that is applied widely, favorable reproducibility detects the method for pre-treatment.
Summary of the invention
Object of the present invention is intended to the defect overcoming prior art, and a kind of phosphate rock floating anionic collector provided detects the method for pre-treatment.
The technical scheme that the method that Collophanite flotation anionic collector of the present invention detects pre-treatment adopts is: containing following processing step:
A. get 10g flotation phosphate ore anionic collector, put into teflon counteracting tank, add 30 ~ 35mL distilled water, regulate solution to pH=2 with dilute sulfuric acid, then add same dilution heat of sulfuric acid 3mL, cover helixseal lid;
B. put into micro-wave oven, effect 10min, takes out and leaves standstill 2 ~ 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL;
C. a large amount of hot distilled water washing, is washed till solution ph 6.8 ~ 7, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.
Teflon counteracting tank described in step a is FR-50 type; Regulate aqueous solution to be measure the commercially available AR level concentrated sulphuric acid to add same volume distilled water formulated with dilute sulfuric acid, the volume ratio of the concentrated sulphuric acid and distilled water is 1:1; Adding dilution heat of sulfuric acid consistent with adjustment dilute sulfuric acid concentration, is same solution; PH=2 accurate pH test paper or pH meter detect and draw.
Microwave power 500W described in step b, is equivalent to household microwave oven power moderate heat.
A large amount of hot distilled waters described in step c refer to the distilled water of boiling; Washing hot distilled water such as volume will exceed container volume, and the lower layer of water after an evacuation container layering abandons; PH value accurate pH test paper or pH meter detect and draw.
Its mechanism is: microwave neither produces reflection to Cucumber and also do not absorbed but pass through smoothly, has instant heat effect, can reach uniform temperature at short notice to absorbent material.This is because microwave makes polar molecule thermal agitation rub with the frequency of 24.5 hundred million times per second, meanwhile, because heated material constantly stirs in the electromagnetic field of high frequency of microwave, greatly strengthen diffusion process, sample is fully reacted, accelerates reaction process, reaction is completed at short notice.Microwave energy, by metallic reflection, can penetrate pottery, glass, teflon, teflon etc., and the material penetrated does not absorb microwave, do not produce heat, only exist as carrier, thus microwave does not have conduction loss, the thermal efficiency is high, and use microwave energy obtains the effect that usual equipment does not reach.Microwave is used for organic chemical reactions as a kind of new form of energy, a lot of reaction in the past can not carried out and be difficult to carry out can not only be made smooth, and it is better than traditional stirring, external heating method greatly as a kind of convenience, rapid, effective, safe mode.
Flotation phosphate under sour environment and microwave action is mining, and anionic collector processing procedure is:
RCOOCH
3+H
2O=RCOOH+CH
3OH
The invention has the beneficial effects as follows:
A. microwave penetrates in teflon material, and mixed solution is fully reacted and reacts evenly, the counteracting tank that this material makes can as the good carrier of microwave heating.
B. microwave makes polar molecule thermal agitation rub with the frequency of 24.5 hundred million times per second, in counteracting tank, mixed solution constantly stirs in the electromagnetic field of high frequency of microwave, greatly strengthen diffusion process, the commercially available phosphate rock floating anionic collector sample containing a small amount of moisture can absorb microwave, accelerate reaction process, reaction is completed at short notice.
C. microwave heating is compared with the traditional approach of external heat with outer stirring: method applicability is strong, and microwave action is simple to operate, and odorless taste; The pre-treatment that microwave heating completes one group of mixed solution needs 15 ~ 20min, and the pre-treatment adopting traditional approach to complete one group of mixed solution needs more than 1h, and operating process is quick, is especially applicable to batch sample process, practicality and replicability strong.
With the collecting agent after the above-mentioned two kinds of mode pre-treatments of gas chromatography determination, error is less, and result is accurate.、
Being also advantageous in that of the inventive method: the activity being increased reactant by microwave, with low cost, avoid causing the pollution to environment, pre-treatment producing equipment need not be detected to existing flotation collophanite stone anionic collector and carry out large change and adjustment, and High Temperature High Pressure ventilation equipment are not needed in course of reaction, simplify technique and cost, with major component composition in gas chromatography determination flotation collophanite stone anionic collector, find that microwave action and classic method gained rock phosphate in powder flotation collector form consistent and each component concentration error less, method simply saves time, cost is low, result is accurate, be convenient to promote, especially the quick detection pre-treatment of batch flotation collophanite stone anionic collector is applicable to, there is certain practical value, composition for flotation collophanite stone anionic collector detects and have found a quick pretreatment method.
Accompanying drawing explanation
Fig. 1 is present invention process process flow diagram;
Fig. 2 is the commercially available rock phosphate in powder flotation collector white plastic fat chromatogram of a kind of direct flotation;
Fig. 3 is the brown plastic fat chromatogram of the commercially available phosphorus ore anionic collector of a kind of reverse flotation;
Fig. 4 is the brown plastic fat chromatogram of the commercially available phosphorus ore anionic collector of another kind of reverse flotation.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited to embodiment.In an embodiment, apart from special instruction, all percentage compositions are mass percent.
The method that a kind of phosphate rock floating anionic collector of the present invention detects pre-treatment is:
A. get 10g flotation phosphate ore anionic collector, put into teflon counteracting tank, add 30 ~ 35mL distilled water, regulate solution to pH=2 with dilute sulfuric acid, then add same dilution heat of sulfuric acid 3mL, cover helixseal lid;
B. put into micro-wave oven, effect 10min, takes out and leaves standstill 2 ~ 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL;
C. a large amount of hot distilled water washing, is washed till solution ph 6.8 ~ 7, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.
Teflon counteracting tank described in step a is FR-50 type (Chengdu Ao Pule Instrument Ltd.); ; Regulate aqueous solution to be measure the commercially available AR level concentrated sulphuric acid to add same volume distilled water formulated with dilute sulfuric acid, the volume ratio of the concentrated sulphuric acid and distilled water is 1:1; Adding dilution heat of sulfuric acid consistent with adjustment dilute sulfuric acid concentration, is same solution; PH=2 accurate pH test paper or pH meter detect and draw.
Microwave power 500W described in step b, is equivalent to household microwave oven power moderate heat.
A large amount of hot distilled waters described in step c refer to the distilled water of boiling; Washing hot distilled water such as slurry volume will exceed container volume, and the lower layer of water after an evacuation container layering abandons; PH value accurate pH test paper or pH meter detect and draw.
Embodiment 1
A. 10g direct flotation rock phosphate in powder anionic collector is got, put into teflon counteracting tank, add 30mL distilled water, with dilute sulfuric acid (1:1---measure the commercially available AR level concentrated sulphuric acid add same volume distilled water formulated), regulate solution to pH=2, add same dilution heat of sulfuric acid 3mL again, cover helixseal lid.
B. put into micro-wave oven, microwave power 500W, effect 10min, takes out and leaves standstill 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL.
C. a large amount of hot distilled water washing, is washed till solution ph 6.9, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.
When d. detecting, inclination liquid-transfering gun draws upper strata oily solution in band plug small test tube, adds a little anhydrous sodium sulfate (about 0.1g), cover plug, for a moment, press GB/T15687-2008 animal and plant fat fatty acid methyl ester preparation method preparation after leaving standstill 1min, gas chromatograph detects in jolting.
Teflon counteracting tank described in step a is FR-50 type (Chengdu Ao Pule Instrument Ltd.); Dilute sulfuric acid regulates aqueous solution to be measure the commercially available AR level concentrated sulphuric acid to add same volume distilled water formulated, and the volume ratio of the concentrated sulphuric acid and distilled water is 1:1; Adding dilution heat of sulfuric acid consistent with adjustment dilute sulfuric acid concentration, is same solution; PH=2 accurate pH test paper or pH meter detect and draw.
Microwave power 500W described in step b, is equivalent to household microwave oven power moderate heat.
A large amount of hot distilled waters described in step c refer to the distilled water of boiling; Washing hot distilled water volume will be as exceeded container volume, and the lower layer of water only extracting solution layering after leaving standstill abandons; PH value accurate pH test paper or pH meter detect and draw.
The a little anhydrous sodium sulfate (about 0.1g) that adds described in steps d is to absorb residual moisture.
In view of the highly confidential property of our company's research and development Collophanite flotation flotation collector composition, select several rock phosphate in powder anionic collector on sale in a large number on the market as data published object.Do the demonstration in method here.
Fig. 2 is the commercially available a kind of direct flotation phosphorus ore anionic collector gained gas chromatogram (Traditional Method gas chromatogram is no longer listed here, has a large amount of announcement on the net) of microwave action:
Table 1 direct flotation commercially available rock phosphate in powder flotation collector white plastic fat component list (area normalization number percent)
Achieve good separation to the commercially available rock phosphate in powder flotation collector fatty acid methyl ester of a kind of direct flotation under this experiment microwave action as seen from Figure 2, microwave action pre-treatment acquired results and Traditional Method result are all within error range.
Embodiment 2
A. get 10g reverse flotation rock phosphate in powder anionic collector, put into teflon counteracting tank, add 30mL distilled water, regulate solution to pH=2 with dilute sulfuric acid (1:1), then add above-mentioned 3mL dilution heat of sulfuric acid, cover helixseal lid.
B. put into micro-wave oven, microwave power 500W, effect 10min, takes out and leaves standstill 2min, and inclination liquid-transfering gun draws upper strata oily solution 3mL.
C. a large amount of hot distilled water washing, is washed till solution ph 7, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.
When d. detecting, inclination liquid-transfering gun draws upper strata oily solution in band plug small test tube, adds a little anhydrous sodium sulfate (about 0.1g), cover plug, for a moment, press GB/T15687-2008 animal and plant fat fatty acid methyl ester preparation method preparation after leaving standstill 1min, gas chromatograph detects in jolting.
Fig. 3 is the commercially available a kind of flotation phosphate ore inverse flotation anionic collector gained gas chromatogram of microwave action:
Table 2 reverse flotation commercially available rock phosphate in powder flotation collector white plastic fat component list (area normalization number percent)
Achieve good separation to the commercially available rock phosphate in powder flotation collector fatty acid methyl ester of a kind of reverse flotation under this experiment microwave action as seen from Figure 3, microwave action pre-treatment acquired results and Traditional Method result are all within error range.
Embodiment 3
A. get 10g flotation phosphate ore anionic collector, put into teflon counteracting tank, add 30mL distilled water, regulate solution to pH=2 with dilute sulfuric acid (1:1), then add above-mentioned 3mL dilution heat of sulfuric acid, cover helixseal lid.
B. put into micro-wave oven, microwave power 500W, effect 10min, takes out and leaves standstill 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL.
C. a large amount of hot distilled water washing, is washed till solution ph 6.8, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by.
When d. detecting, inclination liquid-transfering gun draws upper strata oily solution in band plug small test tube, adds a little anhydrous sodium sulfate (about 0.1g), cover plug, for a moment, press GB/T15687-2008 animal and plant fat fatty acid methyl ester preparation method preparation after leaving standstill 1min, gas chromatograph detects in jolting.
The another kind of reverse flotation brown plastic fat chromatogram of commercially available phosphorus ore anionic collector of Fig. 4.
The another kind of reverse flotation of table 3 commercially available rock phosphate in powder flotation collector white plastic fat component list (area normalization number percent).
Achieve good separation to the commercially available rock phosphate in powder flotation collector fatty acid methyl ester of another kind of reverse flotation under this experiment microwave action as seen from Figure 4, microwave action pre-treatment acquired results and Traditional Method result are all within error range.
In above-mentioned 3 embodiments, change commercially available rock phosphate in powder flotation collecting agent kind (a kind of direct flotation use, two kinds of reverse flotations are used), gained measurement result and employing classic method are caught agent to commercially available three kinds of rock phosphate in powder flotation negative ion and are taken in row contrast, gained fatty acid composition is consistent and each content of fatty acid difference is less, all within permissible error (tolerance 3%), in like manner microwave action method can be used for the pre-treatment that flotation collophanite stone anionic collector detects to acquired results.
Embodiment 4: get 10g flotation collophanite stone anionic collector, put into teflon counteracting tank, add 30 ~ 35mL distilled water, regulate solution to pH=2 with dilute sulfuric acid (1:1), then add above-mentioned 3mL dilution heat of sulfuric acid; Cover helixseal lid, put into micro-wave oven, microwave power 500W, effect 10min, take out and leave standstill 2 ~ 3min, inclination liquid-transfering gun draws upper strata oily solution 3mL, a large amount of hot distilled water washing, be washed till solution ph 6.8 ~ 7, obtain neutral oily solution, draw 1mL to be detected.The present invention have easy, quick, cost is low, the feature such as easy to operate.
Other description of Related Art:
Methyl esterification of fatty acid method
Prepare by GB/T15687-2008 animal and plant fat fatty acid methyl ester preparation method
Chromatographic condition
Chromatographic column (BPX-70 fatty acid analysis dedicated columns, 30m × 320 μm × 0.5 μm); Nitrogen (99.999%) is carrier gas, flow velocity 1.5mL/min; Pressure 0.171MPa before post, injector temperature 250 DEG C, split ratio 50:1; Column temperature: 210 DEG C (keeping 9min); Tail blows 1.5mL/min.
Claims (3)
1. Collophanite flotation detects a method for pre-treatment with anionic collector, it is characterized in that containing following processing step:
(a). get 10g flotation phosphate ore anionic collector, put into teflon counteracting tank, add 30 ~ 35mL distilled water, regulate solution to pH=2 with dilute sulfuric acid, then add same dilution heat of sulfuric acid 3mL, cover helixseal lid;
(b). put into micro-wave oven, effect 10min, takes out and leaves standstill 2 ~ 3min, and inclination liquid-transfering gun draws upper strata oily solution 3mL;
(c). a large amount of hot distilled water washing, is washed till solution ph 6.8 ~ 7, obtains neutral oily solution, draws upper strata oily solution 1mL in tool plug small test tube, covers plug stand-by;
Teflon counteracting tank described in described step (a) is FR-50 type; Regulate aqueous solution to be measure the commercially available AR level concentrated sulphuric acid to add same volume distilled water formulated with dilute sulfuric acid, the volume ratio of the concentrated sulphuric acid and distilled water is 1:1; Adding dilution heat of sulfuric acid consistent with adjustment dilute sulfuric acid concentration, is same solution; PH=2 accurate pH test paper or pH meter detect and draw.
2. Collophanite flotation anionic collector according to claim 1 detects the method for pre-treatment, it is characterized in that: the described microwave power 500W of step (b).
3. Collophanite flotation anionic collector according to claim 1 detects the method for pre-treatment, it is characterized in that: a large amount of hot distilled waters described in step (c) refer to the distilled water of boiling; Washing hot distilled water such as volume will exceed container volume, and the lower layer of water after an evacuation container layering abandons; PH value accurate pH test paper or pH meter detect and draw.
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| CN107167553A (en) * | 2017-06-30 | 2017-09-15 | 云南磷化集团有限公司 | A kind of assay method for determining phosphorus ore anionic collector finished product iodine number |
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| CN101450957A (en) * | 2008-12-31 | 2009-06-10 | 天津科技大学 | Method for synthesizing maltose fatty acid ester by microwave |
| CN101799459A (en) * | 2010-03-31 | 2010-08-11 | 天水师范学院 | Method for measuring phosphorus content of polysaccharide phosphate ester |
| CN102285865B (en) * | 2010-11-16 | 2014-04-16 | 大连天宝化学工业有限公司 | Method for preparing methanol by directly oxidizing methane in ionic liquid under action of microwaves |
| CN102323327B (en) * | 2011-06-15 | 2013-01-30 | 中国地质科学院矿产综合利用研究所 | Method for measuring inductively coupled plasma mass spectrum by carrying out microwave digestion on platinum group element antimony |
| CN102809614A (en) * | 2012-07-18 | 2012-12-05 | 云南磷化集团有限公司 | Method for quickly analyzing phosphorus ore flotation collecting agent |
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