CN105199857A - Method for improving yield of biodiesel - Google Patents
Method for improving yield of biodiesel Download PDFInfo
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- CN105199857A CN105199857A CN201410290721.0A CN201410290721A CN105199857A CN 105199857 A CN105199857 A CN 105199857A CN 201410290721 A CN201410290721 A CN 201410290721A CN 105199857 A CN105199857 A CN 105199857A
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The invention discloses a method for improving the yield of biodiesel. The method comprises the steps that a contact reaction is performed on grease, monohydric alcohol and acidic materials on the conditions that the temperature is set at 100 DEG C-300 DEG C, and the pressure is set at 0.2-10 MPa. According to the method, the yield of the biiodiesel can be improved; in addition, due to the fact that the grease with a high acid value and the high impurity content is treated by taking the acidic materials as a catalyst and cooperating with the certain temperature and pressure, the biodiesel can be prepared at the high yield. Meanwhile, in the method, pretreating (such as pre-esterification treating) does not need to be performed on the grease, so that the biodiesel preparation process is simplified and then the production efficiency is greatly improved.
Description
Technical field
The present invention relates to a kind of method improving biofuel yield.
Background technology
Biofuel is carried out transesterification reaction by grease and monohydroxy-alcohol and is obtained, and has fatty acid ester (i.e. biofuel), in addition mono-glycerides, two sweet esters, glycerine in reaction product, and unreacted alcohol and grease (i.e. triglyceride level).In prior art, the preparation method of biofuel can be divided into acid catalyzed process, base catalysis method, enzyme catalysis method and supercritical methanol technology.
In method disclosed in DE3444893, with acid catalyst, normal pressure, 50-120 DEG C, carries out esterification by free fatty acids and alcohol, carries out pre-esterification process to oil plant, then under base metal catalysts, carry out transesterification reaction, but the acid catalyst left over will be neutralized by alkali, the amount of base metal catalysts can increase.Adopt pre-esterification, make work flow elongated, facility investment, energy consumption significantly rises, and in addition, basic catalyst need be removed from product, has a large amount of waste water to produce, and more difficult recovery glycerine.
CN1031070C adopts pre-esterification-base catalysis method, is first catalyzer with the vitriol oil, phosphoric acid or tosic acid, toluenesulphonic acids and naphthene sulfonic acid, by oil plant and alcohol under 80-160 DEG C of condition, in the tank reactor that band stirs, carries out pre-esterification reactor.After having reacted, add alcohol and excess base, with an acidic catalyst and residual free fatty acids first, residue alkali is as catalyst for ester exchange reaction.
Acid catalysis pre-esterification-base catalysis technique Problems existing compared with base catalysis is that acid catalyst usage quantity is large, is generally the 1-3 % by weight of oil plant, even more, a large amount of spent acid serious environment pollution.Sulfuric acid as esterifying catalyst, in order to reduce the acid number of high-acid-value material.Pre-esterifying process makes work flow elongated, facility investment, and energy consumption increases.
JP9-235573 discloses edible oil that a kind of use discards and methyl alcohol prepares diesel-fuel under the existence of sodium hydroxide, but in natural fats and oils, usually containing free fatty acids, when free fatty acids is more, use base metal catalysts, can produce fatty acid soaps, such base metal catalysts is wanted excessive and is made lipid acid ester layer be separated the difficulty of change with glycerin layer.Base-catalyzed transesterification technique Problems existing needs a basic catalyst to remove from product after reaction, has a large amount of waste water to produce, reclaim glycerine difficulty.
In method disclosed in US5713965A, under the existence of lipase, hexane makes solvent, and grease and alcohol reaction prepare fatty acid methyl ester, i.e. diesel-fuel.
In method disclosed in CN1472280A, using fatty acid ester as acyl acceptor, under the existence of biological enzyme, catalysis biological carries out transesterification reaction production biofuel.Adopt enzyme catalyst exist deficiency be: long reaction time, efficiency are lower, and enzyme catalyst cost is higher, and in high purity methanol easy in inactivation.
JP9905431 discloses a kind of method being prepared fatty acid ester by grease and monohydroxy-alcohol reaction, the method comprises reacts to obtain fatty acid ester by methyl alcohol and grease, at 270-280 DEG C, under 11-12MPa condition, fatty acid methyl ester production rate is 55-60%, can find out, adopt the middle and high platen press of continuous print, still there is the problem that fatty acid ester yield is lower.
Summary of the invention
The present invention, in order to overcome the above-mentioned defect in the preparation method of existing biofuel, provides a kind of method preparing biofuel newly, and the method technical process is simple and can improve the yield of biofuel.
To achieve these goals, the invention provides a kind of method improving biofuel yield, the method comprises makes grease, monohydroxy-alcohol and acid material contact reacts, and described catalytic condition comprises: temperature is 100-300 DEG C, and pressure is 0.2-10MPa.
Method of the present invention can improve the yield of biofuel, and, owing to using acid material as catalyzer, and coordinate certain temperature and pressure, to high acid value and the grease of high impurity content process, still can prepare biofuel by high yield.Meanwhile, in method provided by the invention, do not need to carry out pre-treatment (as pre-esterification process) to described grease, thus simplify the process of preparation biofuel, therefore, substantially increase production efficiency.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The method of raising biofuel yield provided by the invention comprises makes grease, monohydroxy-alcohol and acid material contact reacts, and described catalytic condition comprises: temperature is 100-300 DEG C, and pressure is 0.2-10MPa.
In the present invention, described grease can be the grease of various routine, and its main component is fatty acid triglycercide and/or lipid acid, such as, described grease can be at least one in Vegetable oil lipoprotein, animal grease and microbial oil, can also be frying oil and/or rotten waste oil in addition.Described Vegetable oil lipoprotein such as can comprise soybean oil, rapeseed oil, peanut oil, wunflower seed oil, plam oil, Oleum Cocois and come from the material (comprising the tall oil produced in paper-making process) containing fatty group of the fruit of other various farm crop and wild plant, stem, leaf, limb and root.Animal grease such as can comprise lard, butter, sheep oil, fish oil etc.
In the present invention, described monohydroxy-alcohol can be the monohydroxy-alcohol of carbonatoms between 1-6, can be saturated alcohol, also can be unsaturated alcohol.Under preferable case, described monohydroxy-alcohol is at least one in methyl alcohol, ethanol, propyl alcohol, vinyl carbinol, butanols and amylalcohol, more preferably methyl alcohol and/or ethanol.Described propyl alcohol can be n-propyl alcohol and/or Virahol, and described butanols can be the isomer of propyl carbinol and/or propyl carbinol, and described amylalcohol can be the isomer of Pentyl alcohol and/or Pentyl alcohol.
In the present invention, as long as described grease contacts the yield that can improve biofuel with monohydroxy-alcohol with acid material in aforementioned temperature with pressure range, described acid material refers to the material that can provide hydrogen ion and/or provide L acid, preferably can provide hydrionic material.Under preferable case, described acid material comprises mineral acid and/or mineral acid oil plant.For 100 weight part greases, the consumption of described acid material can be more than 0.001 weight part (as 0.001-50 weight part).
When acid material is mineral acid, to the amount of the acid material added, there is no particular limitation.Under preferable case, relative to the grease of 100 weight parts, the consumption of described mineral acid is 0.001-1 weight part, is more preferably 0.004-0.5 weight part, more preferably 0.01-0.3 weight part, most preferably is 0.02-0.3 weight part.
In the present invention, the acidity in acid material can from B acid and/or L sour, but be preferably B acid, described mineral acid is the conventional various mineral acids in this area, and under preferable case, described mineral acid is at least one in hydrochloric acid, sulfuric acid and phosphoric acid.
In the present invention, when acid material is mineral acid oil plant, to the amount of the acid material added, there is no particular limitation.Under preferable case, relative to the grease of 100 weight parts, consumption >=5 weight part of described mineral acid oil plant, is preferably 5-50 weight part, is more preferably 10-30 weight part.
Hydrogen ion in described mineral acid oil plant can by inorganics contained in oil plant and/or organism ionizes and/or hydrolysis obtains, preferably, in described mineral acid oil plant hydrionic content be 0.001-10mg/100g (namely, in 100g mineral acid oil plant, hydrionic amount is 0.001-10mg), be more preferably 0.01-6mg/100g, more preferably 0.1-4mg/100g, most preferably is 0.1-2mg/100g.According to the preferred embodiment of the present invention, only need containing the hydrogen ion of trace in described mineral acid oil plant, this can make etching problem be solved significantly.
In the present invention, " hydrogen ion content " is recorded by conventional method, such as, can the method for sodium hydroxide titration be adopted to record after being mixed with water by oil plant, not repeat them here.
Described mineral acid oil plant refers to impure acid oil plant (i.e. the mixture of fatty acid triglycercide and/or lipid acid and impurity), wherein impurity can comprise acidic substance (as organic acid and/or mineral acid), other impurity can also be comprised, as one or more in P contained compound, sulfocompound, nitrogenous compound, metallic material, inorganic acid salt, organic acid salt (such as the metal fatty acid salt such as sodium soap, lipid acid potassium) and VITAMIN etc.Lipid acid and above-mentioned impurity can improve the activity of mineral acid oil plant further, often use to have acidity and the biofuel yield of lipid acid and/or the higher grease of foreign matter content or acid oil plant is higher.Lipid acid and/or the higher acid oil plant of foreign matter content are added in active lower grease (such as, foregoing Vegetable oil lipoprotein, animal grease or microbial oil), the yield of biofuel can be improved more significantly.Therefore, the content of the saponifiable matter in described mineral acid oil plant preferably≤97 % by weight (as 85-95 % by weight).It should be noted that, in the present invention, " saponifiable content " refers to the summation of both lipid acid in oil plant and fatty acid triglycercide content.
The acid number of described mineral acid oil plant can be 1-200mgKOH/g, is preferably 30-200mgKOH/g, is more preferably 70-150mgKOH/g.
In the present invention, described grease is different from described mineral acid oil plant usually, and in other words, the hydrogen ion content at least described grease is different from the hydrogen ion content in mineral acid oil plant.Preferably, the hydrogen ion content in described grease is lower than the hydrogen ion content in mineral acid oil plant.
In the inventive method, the weight ratio of monohydroxy-alcohol and grease can in very large range change, and methyl alcohol makes Methanol Recovery amount significantly increase with the too high meeting of weight ratio of oil, and plant energy consumption and process cost increase, and the utilization ratio of equipment is declined.So the weight ratio of grease and monohydroxy-alcohol can be 1:0.05-1, be preferably 1:0.1-0.7, be more preferably 1:0.2-0.7.
The preparation that described contact reacts can carry out biofuel well known by persons skilled in the art and meeting in the reactor of aforementioned temperature and pressure range is carried out, described reactor can be tubular reactor, also can be tank reactor (as autoclave).
When adopting tank reactor, described reactor, preferably with whipping appts, like this, is more conducive to the yield improving biofuel.When carrying out the contact reacts of grease, monohydroxy-alcohol and acid material, described grease, monohydroxy-alcohol and acid material can be provided to reactor separately, are provided to reactor after also can mixing.
When adopting tubular reactor, grease and monohydroxy-alcohol can be supplied to reactor separately, or be supplied to reactor by after their pre-mixings.Preferably, controlling liquid hourly space velocity is 0.1-2h
-1, preferred 0.1-1.6h
-1, before being supplied to reactor, with preheater by material preheating, also directly can enter reactor.If employing preheater, can by grease preheating together with after monohydroxy-alcohol difference preheating or mixing.In tubular reactor, grease and monohydroxy-alcohol preferably enter tubular reactor from tubular reactor bottom, and reacting coarse product flows out from tubular reactor upper end.
In catalytic condition, temperature is higher, and reaction conversion ratio is higher, but temperature higher than 300 DEG C time, reaction product is black, has burnt matter to produce, and meanwhile, glycerine also can be caused to decompose; Temperature is lower, can reduce again the yield of biofuel, and therefore, in foregoing temperature range, for tank reactor, temperature is preferably 120-200 DEG C, and for tubular reactor, temperature is preferably 200-300 DEG C, is more preferably 240-300 DEG C.
Equally, improve pressure favourable to reaction, but pressure is too high, the investment of device and process cost is made to improve more, so, in foregoing pressure ranges, for tank reactor (as stirring tank), pressure is preferably 0.4-1.6MPa, makes apparatus system pressure be in low pressure, and this significantly can reduce the expense of fixed investment; For tubular reactor, pressure is preferably 1-8MPa, is more preferably 3-6MPa.In catalytic process, grease carries out esterification and transesterification reaction simultaneously, extends the contact reacts time favourable to reaction yield raising, so the catalytic time is generally 0.7-10 hour, is preferably 1-6 hour, is more preferably 1-4 hour.
In a preferred embodiment, described method provided by the invention also comprises the mixture obtained after contact reacts isolates lipid acid unitary alcohol ester (mixed ester phase, containing fatty acid ester, mono-glycerides, two sweet esters and unreacted triglyceride level etc.), the method of described separation can adopt conventional separation method to implement, such as, the method for underpressure distillation can be adopted to realize.
In further preferred embodiment, described method provided by the invention isolates monohydroxy-alcohol before being also included in the mixture obtained after contact reacts and isolating lipid acid unitary alcohol ester.The method being separated monohydroxy-alcohol can adopt conventional method (as distillation) to realize.Isolated monohydroxy-alcohol can be recycled.
In preferred embodiment, before isolating lipid acid unitary alcohol ester, isolate glycerine after method provided by the invention is also included in the mixture obtained after contact reacts and isolates monohydroxy-alcohol.The method of separation of glycerin can adopt conventional method to realize, such as, can be realized by settlement separate method.Isolated glycerine can be recycled.
According to method provided by the invention, to the acid number of described grease, there is no particular limitation, such as, can be 0.1-200mgKOH/g.Method of the present invention also can prepare biofuel with higher yields when utilizing the grease of high acid value to carry out contact reacts, and therefore, the acid number of described grease can be 60-200mgKOH/g, is more preferably 90-200mgKOH/g." acid number " refers under test conditions, in and the milligram number of potassium hydroxide needed for 1g grease free fatty acid, measure according to the indicator method in GB/T5530-1998 standard.
The present invention is described in detail by the following examples.The raw material used in embodiment, unless stated otherwise, is commercially available prod.And in the examples below, the yield of biofuel is calculated by following formula:
Yield=(quality of the quality/grease of the final biofuel obtained) × 100% of biofuel.
Embodiment 1
Be the soybean oil of 0.3mgKOH/g by 100g acid number, 17g methyl alcohol and 0.02g sulfuric acid add in autoclave together, under the condition of temperature 140 DEG C, pressure 0.7MPa and stirring velocity 200 revs/min, react 3.5 hours, obtain reacting coarse product.Reacting coarse product is distilled, at the bottom of still < 150 DEG C condition under remove methyl alcohol, and methyl alcohol is reclaimed and reuses, leftover materials are isolated glycerine mutually after, mutually underpressure distillation is carried out to the mixed ester obtained, steam material and be biofuel, the yield of biofuel is 93.5%.
Embodiment 2
Biofuel is prepared according to the method for embodiment 1, unlike, sulphuric acid is 0.8g, and the yield of biofuel is 88%.
Embodiment 3
Be that the rapeseed oil of 67mgKOH/g, 17g methyl alcohol and 0.2g sulfuric acid add in autoclave together by 100g acid number, under the condition of temperature 140 DEG C, pressure 0.7MPa and stirring velocity 200 revs/min, react 3.5 hours, obtain reacting coarse product.Reacting coarse product is distilled, at the bottom of still < 150 DEG C condition under remove methyl alcohol, and methyl alcohol is reclaimed and reuses, leftover materials are isolated glycerine mutually after, mutually underpressure distillation is carried out to the mixed ester obtained, steam material and be biofuel, the yield of biofuel is 96%.
Embodiment 4
Be the waste grease of 97mgKOH/g by 100g acid number, 20g methyl alcohol and 0.3g sulfuric acid add in autoclave together, under the condition of temperature 140 DEG C, pressure 0.8MPa and stirring velocity 200 revs/min, react 3.5 hours, obtain reacting coarse product.Reacting coarse product is distilled, at the bottom of still < 150 DEG C condition under remove methyl alcohol, and methyl alcohol is reclaimed and reuses, leftover materials are isolated glycerine mutually after, mutually underpressure distillation is carried out to the mixed ester obtained, steam material and be biofuel, the yield of biofuel is 94.1%.
Embodiment 5
Take acid number as the waste grease of 20mgKOH/g be raw material, add the mineral acid oil plant (hydrogen ion content is 0.12mg/100g, and acid number is 79mgKOH/g, and saponifiable content is 94.7 % by weight) that weight is grease weight 12%, in alcohol oil quality than 0.17, liquid hourly space velocity 1h
-1condition under, mixing oil plant and methyl alcohol continuously enter into tubular reactor from tubular reactor bottom, controlling temperature in reactor is 240 DEG C, pressure is 4MPa, and reacting coarse product, through distilling out unreacted methyl alcohol, carries out reclaiming, reusing, standing separation glycerine phase, underpressure distillation mixed ester phase, steams material and is biofuel, and the yield of biofuel is 64%.
Comparative example 1
Biofuel is prepared according to the method for embodiment 5, unlike, do not add mineral acid oil plant, the yield of biofuel is 51.1%.
Embodiment 6
Take acid number as the waste grease of 46mgKOH/g be raw material (saponifiable content is 95.2 % by weight), (hydrogen ion content is 1mg/100g to add the mineral acid oil plant that weight is grease weight 30%, acid number is 38.7mgKOH/g, saponifiable content is 93.2 % by weight), in alcohol oil quality than 0.17, liquid hourly space velocity 1h
-1condition under, mixing oil plant and methyl alcohol continuously enter into tubular reactor from tubular reactor bottom, controlling temperature in reactor is 260 DEG C, pressure is 6MPa, and reacting coarse product, through distilling out unreacted methyl alcohol, carries out reclaiming, reusing, standing separation glycerine phase, underpressure distillation mixed ester phase, steams material and is biofuel, and the yield of biofuel is 92.8%.
Comparative example 2
Biofuel is prepared according to the method for embodiment 6, unlike, do not add mineral acid oil plant, the yield of biofuel is 57%.
Comparative example 3
Take acid number as the waste grease of 73mgKOH/g be raw material (hydrogen ion content is 0.006mg/100g, and saponifiable content is 95 % by weight), in alcohol oil quality than 0.17, liquid hourly space velocity 1h
-1condition under, oil plant and methyl alcohol continuously enter into tubular reactor from tubular reactor bottom, controlling temperature in reactor is 260 DEG C, pressure is 6MPa, and reacting coarse product, through distilling out unreacted methyl alcohol, carries out reclaiming, reusing, standing separation glycerine phase, underpressure distillation mixed ester phase, steams material and is biofuel, and the yield of biofuel is 64%.
As can be seen from the above embodiments, method of the present invention can significantly improve the yield of biofuel.Comparing embodiment 1 can be found out with the result of embodiment 2, and when the consumption of acid material is in preferable range of the present invention, the yield of biofuel is higher.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. improve a method for biofuel yield, it is characterized in that, the method comprises makes grease, monohydroxy-alcohol and acid material contact reacts, and described catalytic condition comprises: temperature is 100-300 DEG C, and pressure is 0.2-10MPa.
2. method according to claim 1, wherein, described acid material comprises mineral acid and/or mineral acid oil plant.
3. method according to claim 2, wherein, relative to the grease of 100 weight parts, the consumption of described mineral acid is 0.001-1 weight part, is preferably 0.004-0.5 weight part.
4. according to the method in claim 2 or 3, wherein, described mineral acid is at least one in hydrochloric acid, sulfuric acid and phosphoric acid.
5. method according to claim 2, wherein, relative to the grease of 100 weight parts, consumption >=5 weight part of described mineral acid oil plant, is preferably 5-50 weight part.
6. the method according to claim 2 or 5, wherein, in described mineral acid oil plant, hydrionic content is 0.001-10mg/100g, is preferably 0.01-6mg/100g, is more preferably 0.1-4mg/100g, more preferably 0.1-2mg/100g; The acid number of described mineral acid oil plant is 1-200mgKOH/g, is preferably 30-200mgKOH/g, is more preferably 70-150mgKOH/g.
7. method according to claim 1, wherein, the weight ratio of described grease and monohydroxy-alcohol is 1:0.05-1.
8. method according to claim 1, wherein, described contact reacts is carried out in tank reactor, and described catalytic condition comprises: temperature is 120-200 DEG C, and pressure is 0.4-1.6MPa.
9. method according to claim 1, wherein, described contact reacts is carried out in tubular reactor, and described catalytic condition comprises: temperature is 200-300 DEG C, and be preferably 240-300 DEG C, pressure is 1-8MPa, is preferably 3-6MPa.
10. method according to claim 1, wherein, the acid number of described grease is 0.1-200mgKOH/g, is preferably 60-200mgKOH/g, is more preferably 90-200mgKOH/g.
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