CN102847612A - Biodiesel for coal flotation and preparation method of biodiesel - Google Patents
Biodiesel for coal flotation and preparation method of biodiesel Download PDFInfo
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- CN102847612A CN102847612A CN2012100796286A CN201210079628A CN102847612A CN 102847612 A CN102847612 A CN 102847612A CN 2012100796286 A CN2012100796286 A CN 2012100796286A CN 201210079628 A CN201210079628 A CN 201210079628A CN 102847612 A CN102847612 A CN 102847612A
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses biodiesel for coal flotation and a preparation method of the biodiesel and belongs to the technical fields of utilization of waste oil, preparation of biodiesel and preparation and application of coal flotation agents. The biodiesel is characterized in that the content of fatty acid methyl ester in the biodiesel is higher than 63%, the content of fatty acid monoglyceride is lower than 25%, the content of diglyceride is lower than 10%, and the content of triglyceride is lower than 2%. The preparation method comprises the steps that waste oil serves as a raw material, SO42 is loaded through mesopore silicon oxide, mesopore zirconium oxide or porous zirconium oxide, the biodiesel is obtained by catalytic esterification, and the biodiesel can serve as a flotation agent used in coal flotation. The waste oil serves as a raw material in preparation of the biodiesel. The biodiesel is used in the coal flotation, the production cost of the flotation agent can be reduced greatly, a new purpose of the biodiesel is developed, and the biodiesel is non-toxic and innocuous, capable of degrading biologically and is an effective coal flotation agent.
Description
Technical field
A kind of biodiesel for coal flotation of the present invention and preparation method thereof belongs to the utilization of abandoned oil, the preparation of biodiesel and preparation and the application of Floating agent for coal.In particular to a kind of utilize abandoned oil through mesopore super acids material catalytic esterification for the preparation of biodiesel of coal flotation and preparation method thereof.
Background technology
The flotation of coal is by flotation agent cleaned coal and mineral ash content to be separated, thereby obtains the cleaned coal of high-quality.At present the flotation agent used of coal separation industry is commonly petroleum base kerosene or diesel oil and joins secondary octanol foaming agent as collecting agent and use, and flotation effect is to estimate by clean coal yield and cleans ash.Because petroleum resources in short supply uses petroleum base diesel oil or kerosene to make flotation agent and not only make the coal separation production cost soaring, also sulphur content wherein may be updated in the flotation coal and the reduction ature of coal.Therefore in the petroleum-based energy situation with promoting energy-saving and cost-reducing development in short supply, select the flotation agent for coal preparation of environmental protection and reduction flotation cost, to promoting the development of coal flotation, the needs that satisfy coal flotation industry all are of great practical significance.
The advantages such as biodiesel is compared with petroleum diesel, has the flash-point height, stores transportation safety, and self is biodegradable, and is environmentally friendly, and the nuisance content such as sulfur dioxide, sulfide, carbon dioxide are low in its fire emission, meet environmental requirement.Biodiesel replaces petroleum diesel can alleviate the situation of diesel oil supply shortage, and then alleviates oil supply crisis.But, because biodiesel acts as a fuel and requires fatty acid methyl ester greater than 96.5%, so require complex manufacturing, increase production cost, be difficult in marketing.And if biodiesel is applied to a kind of industry not high to the content requirement of fatty acid methyl ester, then can reduce cost, be beneficial to marketing, more meet the requirement of the environmental protection energy.
The preparation of biodiesel is take animal and plant fat as raw material, makes through ester exchange under catalyst action with methyl alcohol or ethanol, and its method has acid-base catalysis method, catalyzed by biological enzyme and supercritical methanol technology.Adopt homogeneous acid or base catalysis biodiesel processed (such as CN1473907A, DE3444893 etc.) to need neutralization to remove catalyst, produce the waste water that contains in a large number salkali waste or spent acid etc., contaminated environment.Therefore, multiphase solid acid or base catalyst become the focus of research, and CN101338215A discloses with V
2O
5Prepare the method for biodiesel Deng solid acid catalyst, but its conversion ratio is 79%～98%.The step that CN101289629A discloses take biomass based sulfonation charcoal as catalyst prepare the method for biodiesel, and the biodiesel of preparation reaches the index of GB/T20828-2007, but its catalyst prepares and affected greatly by raw material.CN101294096A discloses the agent of employing nano-crystal whisker catalysis and has reacted under Ultrasonic Conditions, and productive rate reaches 97%, but the ultrasonic reaction condition of its use is industrial difficult the realization.The suitability for industrialized production of biodiesel depends primarily on the cost of raw oil material simultaneously, and can greatly reduce its production cost with swill oil, trench wet goods abandoned oil as the raw materials for production of biodiesel.CN200610200554.1, CN200610125581.7 and CN200710130710.6 disclose respectively employing ferric trichloride and alkali, the mixture of p-methyl benzenesulfonic acid, butter of tin and the concentrated sulfuric acid and resin catalyst utilize waste grease to prepare the method for biodiesel.Use mainly as fuel with the biodiesel that first-class method is prepared, and yet there are no report as the application of Floating agent for coal.
Summary of the invention
The present invention discloses a kind of biodiesel for coal flotation and preparation method thereof, its purpose be to seek a kind of cheapness, environmental protection and effectively Floating agent for coal to satisfy modern coal flotation industry to the requirement of flotation agent and flotation effect thereof.
A kind of biodiesel for coal flotation of the present invention is characterized in that described fatty acid methyl esters in biodiesel greater than 63%, and fatty acid monoglyceride content is less than 25%, and dialycerides fat acid and esters content is less than 10%, and fatty acid triglyceride content is less than 2%.
The preparation method of above-mentioned a kind of biodiesel for coal flotation, it is characterized in that the method is as raw material take abandoned oil, make biodiesel through catalytic esterification, catalyst wherein is mesopore super acids solid catalyst, and prepared biodiesel can directly be used for the flotation of coal as flotation agent.Its concrete technology is:
1, in the batch reactor that band stirs, pressing molar ratio of methanol to oil 10-20:1 mixes methyl alcohol and abandoned oil, the mesoporous solids super acidic catalyst that adds again 5-10% abandoned oil quality, reaction temperature 120-200 ℃, reaction pressure 0.1-6.5MPa, reaction time 0.5-3h filters out catalyst after the reaction, with the product standing demix.
2, after the product layering in above-mentioned, get upper strata liquid and catalyst and continue to join in the reactor, add again the methyl alcohol with above-mentioned moderate, at 150-200 ℃, react 0.5-1h under the 0.5-4MPa, filter out catalyst after the reaction, with the product standing demix, get upper strata liquid and can obtain biodiesel.
The preparation method of above-mentioned a kind of biodiesel for coal flotation is characterized in that the content of abandoned oil free fatty acid used in the method at 2%-60%, and fatty acid triglyceride content is at 40%-98%.
The preparation method of above-mentioned a kind of biodiesel for coal flotation is characterized in that mesoporous solids super acidic catalyst used in the method is mesoporous silica-zirconia or porous zirconia load SO
4 2-Catalyst, specific area are 200-600 m
2/ g, the aperture is 1.6-6.4nm.
The flotation effect of flotation agent adopts the XFD-1.5 flotation device to estimate, its method is for to join the biodiesel Floating agent for coal in the coal slurry of flotation cell, and coal-water fluid concentration 100g/L, biodiesel consumption are the 0.8kg-3kg/t coal, flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), stir 2min, bubble 3min is scraped in flotation.
A kind of biodiesel for coal flotation of the present invention and preparation method thereof has the following advantages:
(1) biodiesel is applied in the coal flotation, has opened up a new purposes of biodiesel, and biodiesel is no longer only used as power fuel.
(2) the mesopore super acidic catalyst is applied in synthetic coal flotation with in the reaction of biodiesel; And adopt the secondary response mode to control the ratio of product, reach the requirement that the preparation coal flotation is used biodiesel.
(3) biodiesel is applied directly in the coal flotation, to the content requirement of its fatty acid methyl ester low standard-required＞96.5% such as () biodiesel European Union, the production cost of biodiesel flotation agent is reduced, and then reduce the coal flotation cost.
(4) biodiesel is applied in the coal flotation, and the performance of existing collecting agent has again barbotage concurrently, does not need to add foaming agent.Dialycerides fat acid esters and fatty acid monoglyceride in the biodiesel all have the performance of collecting agent and foaming agent, can also reduce the ash content of cleaned coal simultaneously, have significantly selective.
(5) coal flotation biodiesel, itself is nontoxic, biodegradable, promotes the environmental protection development of coal preparation industry.
(6) not only greatly reduce production cost with swill oil, trench wet goods abandoned oil as the raw materials for production of biodiesel, and reduced environmental pollution, realized twice laid.
The specific embodiment
Embodiment 1:
Get free fatty and fatty acid triglyceride content and be respectively 15% and 85% abandoned oil 41.8g and methyl alcohol 27.1g, join in the 100mL batch reactor and mix, add again 4.2g porous super acids SO
4 2-/ ZrO
2(specific area is 220m to catalyst
2/ g, the aperture is 1.9nm and 2.2nm), stirring reaction 3h under 120 ℃, 0.1MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 27.1g methyl alcohol again, at 150 ℃, stirring reaction 1h under the 0.5MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 68.8%, dialycerides fat acid and esters content 6.6%, fatty acid monoglyceride content 24.4%, fatty acid triglyceride 0.2%.
Get Shanxi and collect blue pit coal sample 150.8g(moisture 0.51%, ash content 15.93%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.435g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 92.97%, cleans ash 12.57%, tail coal productive rate 7.03 %, tail coal ash content 64.33 %.
Embodiment 2:
Get free fatty and fatty acid triglyceride content and be respectively 10% and 90% abandoned oil 41.8g and methyl alcohol 22.3g, join in the 100mL batch reactor and mix, add again 2.2g porous super acids SO
4 2-/ ZrO
2(specific area is 220m to catalyst
2/ g, the aperture is 1.9nm and 2.2nm), stirring reaction 1h under 180 ℃, 2.5MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 22.3g methyl alcohol again, at 150 ℃, stirring reaction 0.5h under the 0.5MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 65.8%, dialycerides fat acid and esters content 8.4%, fatty acid monoglyceride content 24.1%, fatty acid triglyceride 1.7%.
Get Shanxi malanite coal sample 151.1g(moisture 0.72%, ash content 23.80%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.18g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 84.74%, cleans ash 11.12%, tail coal productive rate 15.26 %, tail coal ash content 89.55 %.
Embodiment 3:
Get free fatty and fatty acid triglyceride content and be respectively 2% and 98% abandoned oil 41.8g and methyl alcohol 14.8g, join in the 100mL batch reactor and mix, add again 3.6g mesopore super acids SO
4 2-/ ZrO
2-SiO
2(specific area is 450m to catalyst
2/ g, the aperture is 3.9nm), stirring reaction 0.5h under 200 ℃, 4.8MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 14.8g methyl alcohol again, at 200 ℃, stirring reaction 0.5h under the 4.0MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 64.1%, dialycerides fat acid and esters content 10.0%, fatty acid monoglyceride content 23.9%, fatty acid triglyceride 2.0%.
Get Huozhou, Shanxi pit coal sample 152.3g(moisture 1.50%, ash content 12.36%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.23g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 93.03%, cleans ash 10.39%, tail coal productive rate 6.97 %, tail coal ash content 33.72 %.
Embodiment 4:
Get free fatty and fatty acid triglyceride content and be respectively 58% and 42% abandoned oil 41.8g and methyl alcohol 29.7g, join in the 100mL batch reactor and mix, add again 4.2g mesopore super acids SO
4 2-/ ZrO
2-SiO
2(specific area is 450m to catalyst
2/ g, the aperture is 3.9nm), stirring reaction 3h under 200 ℃, 6.5MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 29.7g methyl alcohol again, at 200 ℃, stirring reaction 1h under the 4.0MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 86.7%, dialycerides fat acid and esters content 3.3%, fatty acid monoglyceride content 9.8%, fatty acid triglyceride 0.2%.
Get Shanxi the Lushui River peace pit coal sample 150.7g(moisture 0.46%, ash content 30.36%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.33g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 82.09%, cleans ash 19.41%, tail coal productive rate 17.91 %, tail coal ash content 79.57 %.
Embodiment 5:
Get free fatty and fatty acid triglyceride content and be respectively 32% and 68% abandoned oil 41.8g and methyl alcohol 29.0g, join in the 100mL batch reactor and mix, add again 2.1g mesopore super acids SO
4 2-/ ZrO
2-SiO
2(specific area is 450m to catalyst
2/ g, the aperture is 3.9nm), stirring reaction 2.5h under 160 ℃, 1.2MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 29.0g methyl alcohol again, at 200 ℃, stirring reaction 0.5h under the 4.0MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 77.8%, dialycerides fat acid and esters content 5.6%, fatty acid monoglyceride content 15.4%, fatty acid triglyceride 1.2%.
Get Yima, henan Province pit coal sample 151.1g(moisture 0.73%, ash content 22.82%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.14g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 82.96%, cleans ash 10.79%, tail coal productive rate 17.04 %, tail coal ash content 79.61 %.
Embodiment 6:
Press the step of embodiment 5, just with mesopore super acids SO
4 2-/ ZrO
2-SiO
2The quantitative change of catalyst is 3.1g, and reaction temperature becomes 200 ℃, and other conditions are constant, make the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 79.5%, dialycerides fat acid and esters content 5.1%, fatty acid monoglyceride content 14.6%, fatty acid triglyceride 0.8%.
Press the float test step of embodiment 5, condition is constant, floatation clean coal productive rate 83.77%, cleans ash 10.58%, tail coal productive rate 16.23 %, tail coal ash content 79.89 %.
Embodiment 7:
Get free fatty and fatty acid triglyceride content and be respectively 25% and 75% abandoned oil 41.8g and methyl alcohol 29.0g, join in the 100mL batch reactor and mix, add again 3.1g mesopore super acids SO
4 2-/ ZrO
2-SiO
2(specific area is 583m to catalyst
2/ g, the aperture is 6.2nm), stirring reaction 2.5h under 160 ℃, 1.2MPa filters out catalyst, with the product standing demix after the reaction.Get upper strata liquid and catalyst and continue to join in the reactor, add 29.0g methyl alcohol again, at 170 ℃, stirring reaction 1h under the 1.2MPa filters out catalyst again, with the product standing demix, gets upper strata liquid and namely gets the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 73.6%, dialycerides fat acid and esters content 6.5%, fatty acid monoglyceride content 20.5%, fatty acid triglyceride 0.4%.
Get Taiyuan Coal Preparation Plant coal sample 156.1g(moisture 3.87%, ash content 20.34%), adopt the XFD-1.5 flotation device to carry out flotation, coal-water fluid concentration 100g/L joins 0.45g coal flotation biodiesel in the coal slurry of flotation cell, stirs 2min, transfer flotation device rotating speed 1800r/min, aeration quantity 0.25m
3/ (m
2Min), bubble 3min is scraped in flotation, and cleaned coal and tail coal be vacuum filtration respectively, dry 24h in 75 ℃ of thermostatic drying chambers then, at last fast ashing in Muffle furnace.Floatation clean coal productive rate 85.96%, cleans ash 10.95%, tail coal productive rate 14.04 %, tail coal ash content 75.63 %.
Embodiment 8:
Press the step of embodiment 7, just free fatty and fatty acid triglyceride content are become respectively 57% and 43%, reaction pressure becomes 5MPa, and other conditions are constant, make the coal flotation biodiesel.By analysis, this fatty acid methyl esters in biodiesel is 95.5%, dialycerides fat acid and esters content 1.3%, fatty acid monoglyceride content 3.2%, and fatty acid triglyceride does not detect.
Press the float test step of embodiment 7, condition is constant, floatation clean coal productive rate 88.32%, cleans ash 11.78%, tail coal productive rate 11.68 %, tail coal ash content 80.12 %.
Claims (4)
1. a biodiesel that is used for coal flotation is characterized in that described fatty acid methyl esters in biodiesel greater than 63%, and fatty acid monoglyceride content is less than 25%, and dialycerides fat acid and esters content is less than 10%, and fatty acid triglyceride content is less than 2%.
2. the preparation method of the described a kind of biodiesel for coal flotation of claim 1, it is characterized in that the method is as raw material take abandoned oil, make biodiesel through catalytic esterification, catalyst wherein is mesopore super acids solid catalyst, prepared biodiesel can directly be used for the flotation of coal as flotation agent, its concrete technology is:
(1), in the batch reactor that band stirs, pressing molar ratio of methanol to oil 10-20:1 mixes methyl alcohol and abandoned oil, the mesoporous solids super acidic catalyst that adds again 5-10% abandoned oil quality, reaction temperature 120-200 ℃, reaction pressure 0.1-6.5MPa, reaction time 0.5-3h filters out catalyst after the reaction, with the product standing demix;
(2), after the product layering in above-mentioned (1), getting upper strata liquid and catalyst continues to join in the reactor, add again the methyl alcohol with above-mentioned (1) moderate, at 150-200 ℃, 0.5-4MPa lower reaction 0.5-1h, filter out catalyst after the reaction, with the product standing demix, get upper strata liquid and can obtain biodiesel.
3. according to the preparation method of the described a kind of biodiesel for coal flotation of claim 2, it is characterized in that the content of abandoned oil free fatty acid used in the method at 2%-60%, fatty acid triglyceride content is at 40%-98%.
4. according to the preparation method of the described a kind of biodiesel for coal flotation of claim 2, it is characterized in that mesoporous solids super acidic catalyst used in the method is mesoporous silica-zirconia or porous zirconia load SO
4 2-Catalyst, specific area are 200-600 m
2/ g, the aperture is 1.6-6.4nm.
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| CN108160337A (en) * | 2017-12-27 | 2018-06-15 | 安徽理工大学 | A kind of method that coal slime flotation collector is prepared using agricultural crop straw |
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| CN110918261A (en) * | 2018-09-19 | 2020-03-27 | 中蓝连海设计研究院有限公司 | Flotation coal slime collecting agent and preparation method and application thereof |
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